Development of a ten inch manipulators-based, flexible, broadband two-crystal spectrometer

NASA Astrophysics Data System (ADS)

Steel, A. B.; Dunn, J.; Emig, J.; Beiersdorfer, P.; Brown, G. V.; Shepherd, R.; Marley, E. V.; Hoarty, D. J.

2014-11-01

We have developed and implemented a broadband X-ray spectrometer with a variable energy range for use at the Atomic Weapons Establishment's Orion Laser. The spectrometer covers an energy bandwidth of ˜1-2 keV using two independently mounted, movable Bragg diffraction crystals. Using combinations of cesium hydrogen pthlate, ammonium dihydrogen phosphate, and pentaerythritol crystals, spectra covering the 1.4-2.5, 1.85-3.15, or 3.55-5.1 keV energy bands have been measured. Image plate is used for detection owing to its high dynamic range. Background signals caused by high energy X-rays and particles commonly produced in high energy laser experiments are reduced by a series of tantalum baffles and filters installed between the source and crystal and also between the crystals and detector.

Development of a ten inch manipulators-based, flexible, broadband two-crystal spectrometer.

PubMed

Steel, A B; Dunn, J; Emig, J; Beiersdorfer, P; Brown, G V; Shepherd, R; Marley, E V; Hoarty, D J

2014-11-01

We have developed and implemented a broadband X-ray spectrometer with a variable energy range for use at the Atomic Weapons Establishment's Orion Laser. The spectrometer covers an energy bandwidth of ∼1-2 keV using two independently mounted, movable Bragg diffraction crystals. Using combinations of cesium hydrogen pthlate, ammonium dihydrogen phosphate, and pentaerythritol crystals, spectra covering the 1.4-2.5, 1.85-3.15, or 3.55-5.1 keV energy bands have been measured. Image plate is used for detection owing to its high dynamic range. Background signals caused by high energy X-rays and particles commonly produced in high energy laser experiments are reduced by a series of tantalum baffles and filters installed between the source and crystal and also between the crystals and detector.

High purity low dislocation GaAs single crystals

NASA Technical Reports Server (NTRS)

Chen, R. T.; Holmes, D. E.; Kirkpatrick, C. G.

1982-01-01

Recent advances in GaAs bulk crystal growth using the LEC (liquid encapsulated Czochralski) technique are described. The dependence of the background impurity concentration and the dislocation density distribution on the materials synthesis and growth conditions were investigated. Background impurity concentrations as low as 4 x 10 to the 15th power were observed in undoped LEC GaAs. The dislocation density in selected regions of individual ingots was very low, below the 3000 cm .3000/sq cm threshold. The average dislocation density over a large annular ring on the wafers fell below the 10000/sq cm level for 3 inch diameter ingots. The diameter control during the program advanced to a diameter variation along a 3 inch ingot less than 2 mm.

Evaluation of a LiI(Eu) neutron detector with coincident double photodiode readout

NASA Astrophysics Data System (ADS)

Yang, H.; Menaa, N.; Bronson, F.; Kastner, M.; Venkataraman, R.; Mueller, W. F.

2011-10-01

Previous work showed that enriched 6Li halide scintillation crystal is a good candidate for portable neutron-sensitive detectors. Photodiode readout is a good alternative to PMT in compact devices. These detectors are often required to work in presence of a strong gamma background. Therefore, great discrimination against gamma rays is crucial. Because of the high Q-value of the 6Li(n,α) 3H reaction, the light yield of a neutron capture signal corresponds to 3-4 MeV gamma equivalent in spite of the quenching effect of heavily charged particles. As a result, energy discrimination is quite effective against gamma signals generated in thin crystals. However, direct gamma interactions inside the photodiode can create pulses whose amplitude is large enough to interfere with thermal neutron peak. This study shows an innovative design based on coincident readout to solve this problem. In this design, two photodiodes are attached on both sides of the LiI crystal. The output signal is only accepted when both photodiodes give out coincident output. The method is proved to effectively suppress background in the neutron window in a 420 mR/h 137Cs field down to the level of natural background.

Status of LUMINEU program to search for neutrinoless double beta decay of 100Mo with cryogenic ZnMoO4 scintillating bolometers

NASA Astrophysics Data System (ADS)

Danevich, F. A.; Bergé, L.; Boiko, R. S.; Chapellier, M.; Chernyak, D. M.; Coron, N.; Devoyon, L.; Drillien, A.-A.; Dumoulin, L.; Enss, C.; Fleischmann, A.; Gastaldo, L.; Giuliani, A.; Gray, D.; Gros, M.; Hervé, S.; Humbert, V.; Ivanov, I. M.; Juillard, A.; Kobychev, V. V.; Koskas, F.; Loidl, M.; Magnier, P.; Makarov, E. P.; Mancuso, M.; de Marcillac, P.; Marnieros, S.; Marrache-Kikuchi, C.; Navick, X.-F.; Nones, C.; Olivieri, E.; Paul, B.; Penichot, Y.; Pessina, G.; Plantevin, O.; Poda, D. V.; Redon, T.; Rodrigues, M.; Shlegel, V. N.; Strazzer, O.; Tenconi, M.; Torres, L.; Tretyak, V. I.; Vasiliev, Ya. V.; Velazquez, M.; Viraphong, O.

2015-10-01

The LUMTNEU program aims at performing a pilot experiment on 0ν2β decay of 100Mo using radiopure ZnMoO4 crystals enriched in 100Mo operated as cryogenic scintillating bolometers. Large volume ZnMoO4 crystal scintillators (˜ 0.3 kg) were developed and tested showing high performance in terms of radiopurity, energy resolution and α/β particle discrimination capability. Zinc molybdate crystal scintillators enriched in 100Mo were grown for the first time by the low-thermal-gradient Czochralski technique with a high crystal yield and an acceptable level of enriched molybdenum irrecoverable losses. A background level of ˜ 0.5 counts/(yr keV ton) in the region of interest can be reached in a large detector array thanks to the excellent detectors radiopurity and particle discrimination capability, suppression of randomly coinciding events by pulse-shape analysis, and anticoincidence cut. These results pave the way to future sensitive searches based on the LUMTNEU technology, capable of approachingand exploring the inverted hierarchy region of the neutrino mass pattern.

Direct bonded HOPG - Analyzer support without background source

NASA Astrophysics Data System (ADS)

Groitl, Felix; Kitaura, Hidetoshi; Nishiki, Naomi; Rønnow, Henrik M.

2018-04-01

A new production process allows a direct bonding of HOPG crystals on Si wafers. This new method facilitates the production of analyzer crystals with support structure without the use of additional, background inducing fixation material, e.g. glue, wax and screws. This new method is especially interesting for the upcoming generation of CAMEA-type multiplexing spectrometers. These instruments allow for a drastic performance increase due to the increased angular coverage and multiple energy analysis. Exploiting the transparency of multiple HOPG for cold neutrons, a consecutive arrangement of HOPG analyzer crystals per Q-channel can be achieved. This implies that neutrons travel through up to 10 arrays of analyzer crystals before reaching the analyzer corresponding to their energy. Hence, a careful choice of the fixation method for the analyzer crystals in regards to transparency and background is necessary. Here, we present first results on the diffraction and mechanical performance of direct bonded analyzer crystals.

Point-contact spectroscopic studies on normal and superconducting AFe2As2-type iron-pnictide single crystals

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

Lu, Xin; Park, W.K.; Yuan, H.Q.

2010-04-23

Point-contact Andreev reflection spectroscopy is applied to investigate the gap structure in iron pnictide single-crystal superconductors of the AFe{sub 2}As{sub 2} (A = Ba, Sr) family ('Fe-122'). The observed point-contact junction conductance curves, G(V), can be divided into two categories: one where Andreev reflection is present for both (Ba{sub 0.6}K{sub 0.4})Fe{sub 2}As{sub 2} and Ba(Fe{sub 0.9}Co{sub 0.1}){sub 2}As{sub 2}, and the other with a V{sup 2/3} background conductance universally observed, extending even up to 100 meV for Sr{sub 0.6}Na{sub 0.4}Fe{sub 2}As{sub 2} and Sr(Fe{sub 0.9}Co{sub 0.1}){sub 2}As{sub 2}. The latter is also observed in point-contact junctions on the nonsuperconducting parentmore » compound BaFe{sub 2}As{sub 2} and superconducting (Ba{sub 0.6}K{sub 0.4})Fe{sub 2}As{sub 2} crystals. Mesoscopic phase-separated coexistence of magnetic and superconducting orders is considered to explain distinct behaviors in the superconducting samples. For Ba{sub 0.6}K{sub 0.4}Fe{sub 2}As{sub 2}, double peaks due to Andreev reflection with a strongly sloping background are frequently observed for point contacts on freshly cleaved c-axis surfaces. If normalized using a background baseline and analyzed using the Blonder–Tinkham–Klapwijk model, the data show a gap size of ~ 3.0–4.0 meV with 2Δ{sub 0}/k{sub B}T{sub c} ~ 2.0–2.6, consistent with the smaller gap size reported for the LnFeAsO family ('Fe-1111'). For the Ba(Fe{sub 0.9}Co{sub 0.1}){sub 2}As{sub 2}, the G(V) curves typically display a zero-bias conductance peak.« less

Point-contact spectroscopic studies on normal and superconducting AFe2As2-type iron pnictide single crystals

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

Lu, Xin; Park, W. K.; Yuan, H. Q.

2010-01-01

Point-contact Andreev reflection spectroscopy is applied to investigate the gap structure in iron pnictide single-crystal superconductors of the AFe{sub 2}As{sub 2} (A = Ba, Sr) family (Fe-122). The observed point-contact junction conductance curves, G(V), can be divided into two categories: one where Andreev reflection is present for both (Ba{sub 0.6}K{sub 0.4})Fe{sub 2}As{sub 2} and Ba(Fe{sub 0.9}Co{sub 0.1}){sub 2}As{sub 2}, and the other with a V{sup 2/3} background conductance universally observed, extending even up to 100 meV for Sr{sub 0.6}Na{sub 0.4}Fe{sub 2}As{sub 2} and Sr(Fe{sub 0.9}Co{sub 0.1}){sub 2}As{sub 2}. The latter is also observed in point-contact junctions on the nonsuperconducting parentmore » compound BaFe{sub 2}As{sub 2} and superconducting (Ba{sub 0.6}K{sub 0.4})Fe{sub 2}As{sub 2} crystals. Mesoscopic phase-separated coexistence of magnetic and superconducting orders is considered to explain distinct behaviors in the superconducting samples. For Ba{sub 0.6}K{sub 0.4}Fe{sub 2}As{sub 2}, double peaks due to Andreev reflection with a strongly sloping background are frequently observed for point contacts on freshly cleaved c-axis surfaces. If normalized using a background baseline and analyzed using the Blonder-Tinkham-Klapwijk model, the data show a gap size of {approx} 3.0-4.0 meV with 2{Delta}{sub 0}/k{sub B}T{sub c} {approx} 2.0-2.6, consistent with the smaller gap size reported for the LnFeAsO family (Fe-1111). For the Ba(Fe{sub 0.9}Co{sub 0.1}){sub 2}As{sub 2}, the G(V) curves typically display a zero-bias conductance peak.« less

SABRE: A New NaI(T1) Dark Matter Direct Detection Experiment

NASA Astrophysics Data System (ADS)

Shields, Emily; Xu, Jingke; Calaprice, Frank

SABRE (Sodium-iodide with Active Background REjection) is a new NaI(Tl) experiment designed to test the DAMA/LIBRA claim for a positive WIMP-dark matter annual modulation signal. SABRE will consist of highly pure NaI(Tl) crystals in an active liquid scintillator veto that will be placed deep underground. The scintillator vessel will provide a veto against external backgrounds and those arising from detector components, especially the 3 keV signature from the decay of 40K in the crystal. Through the use of crystal purification techniques and the veto, we aim for a 40K background significantly lower than that of the DAMA/LIBRA experiment. We present our work developing low-background NaI(Tl) crystals using a highly pure NaI powder and the development of the veto.

Graphene as a protein crystal mounting material to reduce background scatter.

PubMed

Wierman, Jennifer L; Alden, Jonathan S; Kim, Chae Un; McEuen, Paul L; Gruner, Sol M

2013-10-01

The overall signal-to-noise ratio per unit dose for X-ray diffraction data from protein crystals can be improved by reducing the mass and density of all material surrounding the crystals. This article demonstrates a path towards the practical ultimate in background reduction by use of atomically thin graphene sheets as a crystal mounting platform for protein crystals. The results show the potential for graphene in protein crystallography and other cases where X-ray scatter from the mounting material must be reduced and specimen dehydration prevented, such as in coherent X-ray diffraction imaging of microscopic objects.

Graphene as a protein crystal mounting material to reduce background scatter

PubMed Central

Wierman, Jennifer L.; Alden, Jonathan S.; Kim, Chae Un; McEuen, Paul L.; Gruner, Sol M.

2013-01-01

The overall signal-to-noise ratio per unit dose for X-ray diffraction data from protein crystals can be improved by reducing the mass and density of all material surrounding the crystals. This article demonstrates a path towards the practical ultimate in background reduction by use of atomically thin graphene sheets as a crystal mounting platform for protein crystals. The results show the potential for graphene in protein crystallography and other cases where X-ray scatter from the mounting material must be reduced and specimen dehydration prevented, such as in coherent X-ray diffraction imaging of microscopic objects. PMID:24068843

Search for double beta processes in {sup 106}Cd with enriched {sup 106}CdWO{sub 4} crystal scintillator in coincidence with four crystals HPGe detector

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

Danevich, F. A., E-mail: danevich@kinr.kiev.ua; Chernyak, D. M.; Mokina, V. M.

2015-10-28

A radiopure cadmium tungstate crystal scintillator, enriched in {sup 106}Cd ({sup 106}CdWO{sub 4}), was used to search for double beta decay processes in {sup 106}Cd in coincidence with an ultra-low background set-up containing four high purity germanium (HPGe) detectors in a single cryostat. The experiment has been completed after 13085 h of data taking. New improved limits on most of the double beta processes in {sup 106}Cd have been set on the level of 10{sup 20}−10{sup 21} yr. Tn particular, the half-life limit on the two neutrino electron capture with positron emission, T{sub 1/2} ≥ 1.8 × 10{sup 21} yr, reachedmore » the region of theoretical predictions.« less

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

Danevich, F. A., E-mail: danevich@kinr.kiev.ua; Boiko, R. S.; Chernyak, D. M.

The LUMTNEU program aims at performing a pilot experiment on 0ν2β decay of {sup 100}Mo using radiopure ZnMoO{sub 4} crystals enriched in {sup 100}Mo operated as cryogenic scintillating bolometers. Large volume ZnMoO{sub 4} crystal scintillators (∼ 0.3 kg) were developed and tested showing high performance in terms of radiopurity, energy resolution and α/β particle discrimination capability. Zinc molybdate crystal scintillators enriched in {sup 100}Mo were grown for the first time by the low-thermal-gradient Czochralski technique with a high crystal yield and an acceptable level of enriched molybdenum irrecoverable losses. A background level of ∼ 0.5 counts/(yr keV ton) in the regionmore » of interest can be reached in a large detector array thanks to the excellent detectors radiopurity and particle discrimination capability, suppression of randomly coinciding events by pulse-shape analysis, and anticoincidence cut. These results pave the way to future sensitive searches based on the LUMTNEU technology, capable of approachingand exploring the inverted hierarchy region of the neutrino mass pattern.« less

Solar axion search technique with correlated signals from multiple detectors

DOE PAGES

Xu, Wenqin; Elliott, Steven R.

2017-01-25

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

Enhanced cooling of Yb:YLF using astigmatic Herriott cell (Conference Presentation)

NASA Astrophysics Data System (ADS)

Gragossian, Aram; Meng, Junwei; Ghasemkhani, Mohammadreza; Albrecht, Alexander R.; Tonelli, Mauro; Sheik-Bahae, Mansoor

2017-02-01

Optical refrigeration of solids requires crystals with exceptional qualities. Crystals with external quantum efficiencies (EQE) larger than 99% and background absorptions of 4×10-4cm-1 have been cooled to cryogenic temperatures using non resonant cavities. Estimating the cooling efficiency requires accurate measurements of the above mentioned quantities. Here we discuss measurements of EQE and background absorption for two high quality Yb:YLF samples. For any given sample, to reach minimum achievable temperatures heat generated by fluorescence must be removed from the surrounding clamshell and more importantly, absorption of the laser light must be maximized. Since the absorption coefficient drops at lower temperatures the only option is to confine laser light in a cavity until almost 100% of the light is absorbed. This can be achieved by placing the crystal between a cylindrical and spherical mirror to form an astigmatic Herriott cell. In this geometry light enters through a hole in the middle of the spherical mirror and if the entrance angle is correct, it can make as many round trips as required to absorb all the light. At 120 K 60 passes and 150 passes at 100K ensures more than 95% absorption of the laser light. 5 and 10% Yb:YLF crystals placed in such a cell cool to sub 90K temperatures. Non-contact temperature measurements are more challenging for such a geometry. Reabsorption of fluorescence for each pass must be taken into account for accurate temperature measurements by differential luminescence thermometry (DLT). Alternatively, we used part of the spectrum that is not affected by reabsorption.

A novel inert crystal delivery medium for serial femtosecond crystallography

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

Conrad, Chelsie E.; Basu, Shibom; James, Daniel

Serial femtosecond crystallography (SFX) has opened a new era in crystallography by permitting nearly damage-free, room-temperature structure determination of challenging proteins such as membrane proteins. In SFX, femtosecond X-ray free-electron laser pulses produce diffraction snapshots from nanocrystals and microcrystals delivered in a liquid jet, which leads to high protein consumption. A slow-moving stream of agarose has been developed as a new crystal delivery medium for SFX. It has low background scattering, is compatible with both soluble and membrane proteins, and can deliver the protein crystals at a wide range of temperatures down to 4°C. Using this crystal-laden agarose stream, themore » structure of a multi-subunit complex, phycocyanin, was solved to 2.5 Å resolution using 300 µg of microcrystals embedded into the agarose medium post-crystallization. The agarose delivery method reduces protein consumption by at least 100-fold and has the potential to be used for a diverse population of proteins, including membrane protein complexes.« less

A novel inert crystal delivery medium for serial femtosecond crystallography

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

Conrad, Chelsie E.; Basu, Shibom; James, Daniel

Serial femtosecond crystallography (SFX) has opened a new era in crystallography by permitting nearly damage-free, room-temperature structure determination of challenging proteins such as membrane proteins. In SFX, femtosecond X-ray free-electron laser pulses produce diffraction snapshots from nanocrystals and microcrystals delivered in a liquid jet, which leads to high protein consumption. A slow-moving stream of agarose has been developed as a new crystal delivery medium for SFX. It has low background scattering, is compatible with both soluble and membrane proteins, and can deliver the protein crystals at a wide range of temperatures down to 4°C. Using this crystal-laden agarose stream, themore » structure of a multi-subunit complex, phycocyanin, was solved to 2.5Å resolution using 300µg of microcrystals embedded into the agarose medium post-crystallization. The agarose delivery method reduces protein consumption by at least 100-fold and has the potential to be used for a diverse population of proteins, including membrane protein complexes.« less

A novel inert crystal delivery medium for serial femtosecond crystallography

DOE PAGES

Conrad, Chelsie E.; Basu, Shibom; James, Daniel; ...

2015-06-30

Serial femtosecond crystallography (SFX) has opened a new era in crystallography by permitting nearly damage-free, room-temperature structure determination of challenging proteins such as membrane proteins. In SFX, femtosecond X-ray free-electron laser pulses produce diffraction snapshots from nanocrystals and microcrystals delivered in a liquid jet, which leads to high protein consumption. A slow-moving stream of agarose has been developed as a new crystal delivery medium for SFX. It has low background scattering, is compatible with both soluble and membrane proteins, and can deliver the protein crystals at a wide range of temperatures down to 4°C. Using this crystal-laden agarose stream, themore » structure of a multi-subunit complex, phycocyanin, was solved to 2.5 Å resolution using 300 µg of microcrystals embedded into the agarose medium post-crystallization. The agarose delivery method reduces protein consumption by at least 100-fold and has the potential to be used for a diverse population of proteins, including membrane protein complexes.« less

Scintillation properties of a 2-inch diameter KCa0.8Sr0.2I3:Eu2+ single crystal

NASA Astrophysics Data System (ADS)

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

2017-09-01

Inch-sized scintillating crystals are required for practical radiation detectors such as hand-held radio-isotope identification devices. In this work, a transparent and colorless 2-inch diameter KCa0.8Sr0.2I3: 0 . 5 mo% Eu2+ single crystal was grown by the vertical Bridgman method, and the scintillation properties of a ∅ 50 mm × 45 mm long sample were evaluated. The Eu2+ 5d1- 4 f emission under X-ray excitation is centered at 472 nm. Its scintillation decay time under 137 Cs source irradiation is 2 . 37 μs, and the absolute light output is 51,000 ± 3000 photons/MeV. The energy resolution at 662 keV was evaluated for different orientations of the crystals with respect to the PMT, and the effect of 40 K background subtraction on energy resolution was evaluated. The performance of the packaged crystal was also investigated.

Sequential changes in biliary lipids and gallbladder ion transport during gallstone formation.

PubMed Central

Giurgiu, D I; Saunders-Kirkwood, K D; Roslyn, J J; Abedin, M Z

1997-01-01

OBJECTIVE: This study sought to correlate gallbladder (GB) Na+ and Cl-) fluxes with biliary lipid composition during the various stages of gallstone (GS) formation. SUMMARY BACKGROUND DATA: GS formation is associated with altered GB ion transport and increased biliary lipid and Ca2+ concentrations. Nonetheless, the longitudinal relationship between ion transport and biliary lipid changes during GS formation has not been defined. METHODS: Prairie dogs were fed standard (n = 18) or 1.2% cholesterol-enriched (n = 30) diets for 4 to 21 days. Hepatic and GB bile were analyzed for lipids and Ca2+. Animals were designated either Pre-Crystal, Crystal, or GS based on absence or presence of crystals or GS, respectively. GBs were mounted in Ussing chambers, electrophysiologic parameters were recorded, and unidirectional Na+ and Cl- fluxes measured. RESULTS: Short-circuit current and potential difference were similar during Pre-Crystal and Crystal stages but significantly reduced during GS stage compared to controls and Pre-Crystals. Transepithelial resistance was similar in all groups. Net Na+ absorption was increased during Pre-Crystal but decreased during GS stage due to increased mucosa-to-serosa and serosa-to-mucosa flux, respectively. Increased serosa-to-mucosa flux of both Na+ and Cl- characterized the Crystal stage. Biliary lipids and Ca2+ increased progressively during various stages of GS formation and correlated positively with unidirectional fluxes of Na+ and Cl-. CONCLUSION: GB epithelial ion transport changes sequentially during GS formation, with the early Pre-Crystal stage characterized by increased Na+ absorption, and the later Crystal stage accompanied by prosecretory stimuli on Na+ and Cl- fluxes, which may be due to elevated GB bile Ca2+ and total bile acids. Images Figure 1. Figure 3. Figure 4. PMID:9114797

Continuous diffraction of molecules and disordered molecular crystals

PubMed Central

Yefanov, Oleksandr M.; Ayyer, Kartik; White, Thomas A.; Barty, Anton; Morgan, Andrew; Mariani, Valerio; Oberthuer, Dominik; Pande, Kanupriya

2017-01-01

The intensities of far-field diffraction patterns of orientationally aligned molecules obey Wilson statistics, whether those molecules are in isolation (giving rise to a continuous diffraction pattern) or arranged in a crystal (giving rise to Bragg peaks). Ensembles of molecules in several orientations, but uncorrelated in position, give rise to the incoherent sum of the diffraction from those objects, modifying the statistics in a similar way as crystal twinning modifies the distribution of Bragg intensities. This situation arises in the continuous diffraction of laser-aligned molecules or translationally disordered molecular crystals. This paper develops the analysis of the intensity statistics of such continuous diffraction to obtain parameters such as scaling, beam coherence and the number of contributing independent object orientations. When measured, continuous molecular diffraction is generally weak and accompanied by a background that far exceeds the strength of the signal. Instead of just relying upon the smallest measured intensities or their mean value to guide the subtraction of the background, it is shown how all measured values can be utilized to estimate the background, noise and signal, by employing a modified ‘noisy Wilson’ distribution that explicitly includes the background. Parameters relating to the background and signal quantities can be estimated from the moments of the measured intensities. The analysis method is demonstrated on previously published continuous diffraction data measured from crystals of photosystem II [Ayyer et al. (2016 ▸), Nature, 530, 202–206]. PMID:28808434

Characterizing Background Events in Neutron Transmutation Doped Thermistors for CUORE-0

NASA Astrophysics Data System (ADS)

Dutta, Suryabrata; Cuore Collaboration

2017-09-01

The Cryogenic Underground Observatory for Rare Events (CUORE) is a ton-scale neutrinoless double-beta decay experiment operating at the Laboratori Nazionali del Gran Sasso (LNGS). The experiment is comprised of 988 TeO2 bolometric crystals arranged into 19 towers and operated at a temperature of 15 mK. A neutron-transmutation-doped (NTD) Ge thermistor measures the thermal response from particles incident on the crystals. However, bulk and surface contamination of the NTD thermistors themselves produce distorted thermal responses inside the thermistor volume. Although these pulses are efficiently removed from the double-beta decay analysis by pulse shape cuts, they can be used to extract information about thermistor contamination. I will present a multifaceted approach to characterize these events, in which I implement an improved hot-electron thermal model, Geant4 Monte Carlo simulations of background events, and data from a previous experiment, CUORE-0, reprocessed with a new optimal filter. Using this approach, rates and energy deposition from contamination inside the NTD thermistors are measured, giving us better understanding of a CUORE background source.

VIEW TO EAST OF CRYSTALLIZATION LABORATORY (CENTER LEFT FOREGROUND), PAINT ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

VIEW TO EAST OF CRYSTALLIZATION LABORATORY (CENTER LEFT FOREGROUND), PAINT APPLICATION BUILDING (CENTER BACKGROUND), AND c1944-1950 c1944-1950 POST-U.S. RADIUM ADDITION ADDITIONS TO EACH BUILDING (RIGHT FOREGROUND AND BACKGROUND) - United States Radium Corporation, 422-432 Alden Street, Orange, Essex County, NJ

Synthesis and solid-state characterisation of 4-substituted methylidene oxindoles

PubMed Central

2013-01-01

Background 4-substituted methylidene oxindoles are pharmacologically important. Detailed analysis and comparison of all the interactions present in crystal structures is necessary to understand how these structures arise. The XPac procedure allows comparison of complete crystal structures of related families of compounds to identify assemblies that are mainly the result of close-packing as well as networks of directed interactions. Results Five 4-substituted methylidene oxindoles have been synthesized by the Knoevenagel condensation of oxindole with para-substituted aromatic aldehydes and were characterized in the solid state by x-ray crystallography. Hence, the structures of (3E)-3-(4-Bromobenzylidene)-1,3-dihydro-2H-indol-2-one, 3a, (3E)-3-(4-Chlorobenzylidene)-1,3-dihydro-2H-indol-2-one, 3b, (3E)-3-(4-Methoxybenzylidene)-1,3-dihydro-2H-indol-2-one, 3c, (3E)-3-(4-Methylbenzylidene)-1,3-dihydro-2H-indol-2-one, 3d and (3E)-3-(4-Nitrobenzylidene)-1,3-dihydro-2H-indol-2-one, 3e, were elucidated using single crystal X-ray crystallography. Conclusions A hydrogen bonded dimer molecular assembly or supramolecular construct was identified in all the crystal structures examined along with a further four 1D supramolecular constructs which were common to at least two of the family of structures studied. The 1D supramolecular constructs indicate that once the obvious strong interaction is satisfied to form hydrogen bonded dimer it is the conventionally weaker interactions, such as steric bulk and edge-to-face interactions which compete to influence the final structure formation. PMID:24517531

Rotation Rate Sensing via Magnetostatic Surface Wave Propagation on a Thick Yig Ring.

DTIC Science & Technology

1979-12-03

Introduction . . . . . . . . . . . 1 Background . . . . . . . . I Statement of the Problem. o o . 4 Plan of Attack. o. . o o o • 4 Sequence of...crystal growth process. It was subsequently suggested that the thin film disfiguration problem could be avoided by ma- chining the desired ring...sensor provide any practical advantages that would make it a better choice over current rate sensing schemes? Plan of Attack This thesis concerns itself

Properties of magnetized Coulomb crystals of ions with polarizable electron background

NASA Astrophysics Data System (ADS)

Kozhberov, A. A.

2018-06-01

We have studied phonon and thermodynamic properties of a body-centered cubic (bcc) Coulomb crystal of ions with weakly polarized electron background in a uniform magnetic field B. At B = 0, the difference between phonon moments calculated using the Thomas-Fermi (TF) and random phase approximations is always less than 1% and for description of phonon properties of a crystal, TF formalism was used. This formalism was successfully applied to investigate thermodynamic properties of magnetized Coulomb crystals. It was shown that the influence of the polarization of the electron background is significant only at κ TF a > 0.1 and T ≪ T p ( 1 + h2 ) - 1 / 2 , where κTF is the Thomas-Fermi wavenumber, a is the ion sphere radius, T p ≡ ℏ ω p is the ion plasma temperature, h ≡ ω B / ω p , ωB is the ion cyclotron frequency, and ωp is the ion plasma frequency.

The quick and ultrasensitive determination of K in NaI using inductively coupled plasma mass spectrometry

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

Arnquist, Isaac J.; Hoppe, Eric W.

A highly sensitive, novel and quick assay method utilizing inductively coupled plasma mass spectrometry was developed for the determination of K in NaI powders and NaI(Tl) scintillator crystals for use in ultralow background applications. The determination of K (viz. 40K), as well as Th and U and their daughters, is important in ultralow background detector materials to ensure incorporation of materials of sufficiently high radiopurity. Through the use of improved instrumentation, cool plasma operating conditions, and meticulously clean sample preparations, detection limits of 11 fg natK∙g-1 (or 341 pBq 40K∙kg-1) was attained for K in pure water. Detection limits inmore » the sample matrix (i.e., NaI) were 0.529 ng natK∙g NaI-1 (or 16.4 Bq 40K∙kg NaI -1). A number of different precursor NaI powder samples and NaI(Tl) scintillator crystals were assayed for their K content. Determinations ranged from 0.757 – 31.4 ng natK∙g NaI-1. This method allows for the screening of materials to unprecedented levels in a fraction of the time compared to gamma counting techniques, providing a useful method for a more effective screening tool of K in ultralow background detector materials.« less

Surface alpha backgrounds from plate-out of radon progeny

NASA Astrophysics Data System (ADS)

Perumpilly, Gopakumar; Guiseppe, Vincente

2012-03-01

Low-background detectors operating underground aim for unprecedented low levels of radioactive backgrounds. Although the radioactive decays of airborne radon (particularly Rn-222) and its subsequent daughters present in an experiment are potential backgrounds, more troublesome is the deposition of radon daughters on detector materials. Exposure to radon at any stage of assembly of an experiment can result in surface contamination by daughters supported by the long half life (22 y) of Pb-210 on sensitive locations of a detector. We have developed a model of the radon progeny implantation using Geant4 simulations based on the low energy nuclear recoil process. We explore the alpha decays from implanted progeny on a Ge crystal as potential backgrounds for a neutrinoless double-beta decay experiment. Results of the simulations validated with alpha spectrum measurement of plate-out samples will be presented.

Effect of background dielectric on TE-polarized photonic bandgap of metallodielectric photonic crystals using Dirichlet-to-Neumann map method.

PubMed

Sedghi, Aliasghar; Rezaei, Behrooz

2016-11-20

Using the Dirichlet-to-Neumann map method, we have calculated the photonic band structure of two-dimensional metallodielectric photonic crystals having the square and triangular lattices of circular metal rods in a dielectric background. We have selected the transverse electric mode of electromagnetic waves, and the resulting band structures showed the existence of photonic bandgap in these structures. We theoretically study the effect of background dielectric on the photonic bandgap.

HEALTH AND SOCIAL HARMS ASSOCIATED WITH CRYSTAL METHAMPHETAMINE USE AMONG STREET-INVOLVED YOUTH IN A CANADIAN SETTING

PubMed Central

Uhlmann, Sasha; DeBeck, Kora; Simo, Annick; Kerr, Thomas; Montaner, Julio S.G.; Wood, Evan

2013-01-01

Background and objectives Despite recent increases in crystal methamphetamine use among high-risk populations such as street-involved youth, few prospective studies have examined the health and social outcomes associated with active crystal methamphetamine use. Methods We enrolled 1,019 street-involved youth in Vancouver, Canada, in a prospective cohort known as the At-Risk Youth Study (ARYS). Participants were assessed semi-annually and a generalized estimating equation (GEE) logistic regression was used to identify factors independently associated with active crystal methamphetamine use. Results Among 1,019 participants recruited into ARYS between 2005 and 2012 the median follow up duration was 17 months, 320 (31.4%) participants were female and 454 (44.6%) had previously used crystal methamphetamine at baseline. In adjusted GEE analyses, active crystal methamphetamine use was independently associated with Caucasian ethnicity (Adjusted Odds Ratio [AOR] = 1.37; 95% Confidence Interval [CI]: 1.04 – 1.81), homelessness (AOR = 1.34; 95% CI: 1.15 – 1.56), injection drug use (AOR = 3.40; 95% CI: 2.76 – 4.19), non-fatal overdose (AOR = 1.46; 95% CI: 1.07 – 2.00), being a victim of violence (AOR = 1.19; 95% CI: 1.02 – 1.38), involvement in sex work (AOR = 1.39; 95% CI: 1.03 – 1.86) and drug dealing (AOR = 1.60; 95% CI: 1.35 – 1.90). Discussion and conclusions Prevalence of crystal methamphetamine use was high in this setting and active use was independently associated with a range of serious health and social harms. Scientific Significance Evidence-based strategies to prevent and treat crystal methamphetamine use are urgently needed. PMID:24628742

Coherent manipulation of dipolar coupled spins in an anisotropic environment

NASA Astrophysics Data System (ADS)

Baibekov, E. I.; Gafurov, M. R.; Zverev, D. G.; Kurkin, I. N.; Malkin, B. Z.; Barbara, B.

2014-11-01

We study coherent dynamics in a system of dipolar coupled spin qubits diluted in a solid and subjected to a driving microwave field. In the case of rare earth ions, an anisotropic crystal background results in anisotropic g tensor and thus modifies the dipolar coupling. We develop a microscopic theory of spin relaxation in a transient regime for the frequently encountered case of axially symmetric crystal field. The calculated decoherence rate is nonlinear in the Rabi frequency. We show that the direction of a static magnetic field that corresponds to the highest spin g factor is preferable in order to obtain a higher number of coherent qubit operations. The results of calculations are in excellent agreement with our experimental data on Rabi oscillations recorded for a series of CaW O4 crystals with different concentrations of N d3 + ions.

Status of the MAJORANA DEMONSTRATOR

NASA Astrophysics Data System (ADS)

Vasilyev, S.; Abgrall, N.; Arnquist, I. J.; Avignone, F. T.; Balderrot-Barrera, C. X.; Barabash, A. S.; Bertrand, F. E.; Bradley, A. W.; Brudanin, V.; Busch, M.; Buuck, M.; Byram, D.; Caldwell, A. S.; Chan, Y.-D.; Christofferson, C. D.; Cuesta, C.; Detwiler, J. A.; Efremenko, Yu.; Ejiri, H.; Elliott, S. R.; Galindo-Uribarri, A.; Gilliss, T.; Giovanetti, G. K.; Goett, J.; Green, M. P.; Gruszko, J.; Guinn, I.; Guiseppe, V. E.; Henning, R.; Hoppe, E. W.; Howard, S.; Howe, M. A.; Jasinski, B. R.; Keeter, K. E.; Kidd, M. F.; Konovalov, S. I.; Kouzes, R. T.; LaFerriere, B. D.; Leon, J.; MacMullin, J.; Martin, R. D.; Meijer, S. J.; Mertens, S.; Orrell, J. L.; O'Shaughnessy, C.; Poon, A. W. P.; Radford, D. C.; Rager, J.; Rielage, K.; Robertson, R. G. H.; Romero-Romero, E.; Shanks, B.; Shirchenko, M.; Snyder, N.; Suriano, A. M.; Tedeschi, D.; Trimble, J. E.; Varner, R. L.; Vetter, K.; Vorren, K.; White, B. R.; Wilkerson, J. F.; Wiseman, C.; Xu, W.; Yakushev, E.; Yu, C.-H.; Yumatov, V.; Zhitnikov, I.

2017-01-01

The MAJORANA Collaboration is constructing the MAJORANA DEMONSTRATOR, an ultralow background, 40-kg modular high purity Ge (HPGe) detector array to search for neutrinoless double-beta decay (0νββ-decay) in 76Ge. The goal of the experiment is to demonstrate a background rate at or below 3 counts/(t-y) in the 4 keV region of interest (ROI) around the 2039 keV Q-value for 76Ge 0νββ-decay. In this paper, the status of the MAJORANA DEMONSTRATOR, including its design and measurements of properties of the HPGe crystals is presented.

Crystal identification for a dual-layer-offset LYSO based PET system via Lu-176 background radiation and mean shift algorithm

NASA Astrophysics Data System (ADS)

Wei, Qingyang; Ma, Tianyu; Xu, Tianpeng; Zeng, Ming; Gu, Yu; Dai, Tiantian; Liu, Yaqiang

2018-01-01

Modern positron emission tomography (PET) detectors are made from pixelated scintillation crystal arrays and readout by Anger logic. The interaction position of the gamma-ray should be assigned to a crystal using a crystal position map or look-up table. Crystal identification is a critical procedure for pixelated PET systems. In this paper, we propose a novel crystal identification method for a dual-layer-offset LYSO based animal PET system via Lu-176 background radiation and mean shift algorithm. Single photon event data of the Lu-176 background radiation are acquired in list-mode for 3 h to generate a single photon flood map (SPFM). Coincidence events are obtained from the same data using time information to generate a coincidence flood map (CFM). The CFM is used to identify the peaks of the inner layer using the mean shift algorithm. The response of the inner layer is deducted from the SPFM by subtracting CFM. Then, the peaks of the outer layer are also identified using the mean shift algorithm. The automatically identified peaks are manually inspected by a graphical user interface program. Finally, a crystal position map is generated using a distance criterion based on these peaks. The proposed method is verified on the animal PET system with 48 detector blocks on a laptop with an Intel i7-5500U processor. The total runtime for whole system peak identification is 67.9 s. Results show that the automatic crystal identification has 99.98% and 99.09% accuracy for the peaks of the inner and outer layers of the whole system respectively. In conclusion, the proposed method is suitable for the dual-layer-offset lutetium based PET system to perform crystal identification instead of external radiation sources.

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

Hull, G; Zaitseva, N; Cherepy, N

Efficient, readily-available, low-cost, high-energy neutron detectors can play a central role in detecting illicit nuclear weapons since neutrons are a strong indication for the presence of fissile material such as Plutonium and Highly-Enriched Uranium. The main challenge in detecting fast neutrons consists in the discrimination of the signal from the gamma radiation background. At present, the only well-investigated organic crystal scintillator for fast neutron detection, in a n/{gamma} mixed field, is stilbene, which while offering good pulse shape discrimination, is not widely used because of its limited availability and high cost. In this work we report the results of ourmore » studies made with a number of new organic crystals, which exhibit pulse shape discrimination for detection of fast neutrons. In particular 1,1,4,4-tetraphenyl-1,3-butadiene features a light yield higher than anthracene and a Figure of Merit (FOM) for the pulse shape discrimination better than stilbene. New crystals are good candidates for the low-cost solution growth method, thus representing promising organic scintillators for widespread deployment for high-energy neutron detection.« less

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

PubMed

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

2015-10-01

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

Investigation of supramolecular synthons and structural characterisation of aminopyridine-carboxylic acid derivatives

PubMed Central

2014-01-01

Background Co-crystal is a structurally homogeneous crystalline material that contains two or more neutral building blocks that are present in definite stoichiometric amounts. The main advantage of co-crystals is their ability to generate a variety of solid forms of a drug that have distinct physicochemical properties from the solid co-crystal components. In the present investigation, five co-crystals containing 2-amino-6-chloropyridine (AMPY) moiety were synthesized and characterized. Results The crystal structure of 2-amino-6-chloropyridine (AMPY) (I), and the robustness of pyridine-acid supramolecular synthon were discussed in four stoichiometry co-crystals of AMPY…BA (II), AMPY…2ABA (III), AMPY…3CLBA (IV) and AMPY…4NBA (V). The abbreviated designations used are benzoic acid (BA), 2-aminobenzoic acid (2ABA), 3-chlorobenzoic acid (3CLBA) and 4-nitrobenzoic acid (4NBA). All the crystalline materials have been characterized by 1HNMR, 13CNMR, IR, photoluminescence, TEM analysis and X-ray diffraction. The supramolecular assembly of each co-crystal is analyzed and discussed. Conclusions Extensive N---H · · · N/N---H · · · O/O---H · · · N hydrogen bonds are found in (I-V), featuring different supramolecular synthons. In the crystal structure, for compound (I), the 2-amino-6-chloropyridine molecules are linked together into centrosymmetric dimers by hydrogen bonds to form homosynthon, whereas for compounds (II-V), the carboxylic group of the respective acids (benzoic acid, 2-aminobenzoic acid, 3-chlorobenzoic acid and 4-nitrobenzoic acid) interacts with pyridine molecule in a linear fashion through a pair of N---H · · · O and O---H · · · N hydrogen bonds, generating cyclic hydrogen-bonded motifs with the graph-set notation R 2 2 8 , to form heterosynthon. In compound (II), another intermolecular N---H · · · O hydrogen bonds further link these heterosynthons into zig-zag chains. Whereas in compounds (IV) and (V), these heterosynthons are centrosymmetrically paired via N---H · · · O hydrogen bonds and each forms a complementary DADA [D = donor and A = acceptor] array of quadruple hydrogen bonds, with graph-set notation R238, R228 and R238. PMID:24887234

Localized rejuvenation of a crystal mush recorded in zircon temporal and compositional variation at the Lassen Volcanic Center, northern California

USGS Publications Warehouse

Klemetti, Erik W.; Clynne, Michael A.

2014-01-01

Zircon ages and trace element compositions from recent silicic eruptions in the Lassen Volcanic Center (LVC) allow for an evaluation of the timing and conditions of rejuvenation (reheating and mobilization of crystals) within the LVC magmatic system. The LVC is the southernmost active Cascade volcano and, prior to the 1980 eruption of Mount St. Helens, was the site of the only eruption in the Cascade arc during the last century. The three most recent silicic eruptions from the LVC were very small to moderate-sized lava flows and domes of dacite (1915 and 27 ka eruptions of Lassen Peak) and rhyodacite (1.1 ka eruption of Chaos Crags). These eruptions produced mixed and mingled lavas that contain a diverse crystal cargo, including zircon. 238U-230Th model ages from interior and surface analyses of zircon reveal ages from ~17 ka to secular equilibrium (>350 ka), with most zircon crystallizing during a period between ~60–200 ka. These data support a model for localized rejuvenation of crystal mush beneath the LVC. This crystal mush evidently is the remnant of magmatism that ended ~190 ka. Most zircon are thought to have been captured from “cold storage” in the crystal mush (670–725°C, Hf >10,000 ppm, Eu/Eu* 0.25–0.4) locally remobilized by intrusion of mafic magma. A smaller population of zircon (>730°C, Hf <10,000 ppm, Eu/Eu* >0.4) grew in, and are captured from, rejuvenation zones. These data suggest the dominant method to produce eruptible melt within the LVC is small-scale, local rejuvenation of the crystal mush accompanied by magma mixing and mingling. Based on zircon stability, the time required to heat, erupt and then cool to background conditions is relatively short, lasting a maximum of 10 s–1000 s years. Rejuvenation events in the LVC are ephemeral and permit eruption within an otherwise waning and cooling magmatic body.

Localized rejuvenation of a crystal mush recorded in zircon temporal and compositional variation at the Lassen Volcanic Center, northern California.

PubMed

Klemetti, Erik W; Clynne, Michael A

2014-01-01

Zircon ages and trace element compositions from recent silicic eruptions in the Lassen Volcanic Center (LVC) allow for an evaluation of the timing and conditions of rejuvenation (reheating and mobilization of crystals) within the LVC magmatic system. The LVC is the southernmost active Cascade volcano and, prior to the 1980 eruption of Mount St. Helens, was the site of the only eruption in the Cascade arc during the last century. The three most recent silicic eruptions from the LVC were very small to moderate-sized lava flows and domes of dacite (1915 and 27 ka eruptions of Lassen Peak) and rhyodacite (1.1 ka eruption of Chaos Crags). These eruptions produced mixed and mingled lavas that contain a diverse crystal cargo, including zircon. 238U-230Th model ages from interior and surface analyses of zircon reveal ages from ∼17 ka to secular equilibrium (>350 ka), with most zircon crystallizing during a period between ∼60-200 ka. These data support a model for localized rejuvenation of crystal mush beneath the LVC. This crystal mush evidently is the remnant of magmatism that ended ∼190 ka. Most zircon are thought to have been captured from "cold storage" in the crystal mush (670-725°C, Hf >10,000 ppm, Eu/Eu* 0.25-0.4) locally remobilized by intrusion of mafic magma. A smaller population of zircon (>730°C, Hf <10,000 ppm, Eu/Eu* >0.4) grew in, and are captured from, rejuvenation zones. These data suggest the dominant method to produce eruptible melt within the LVC is small-scale, local rejuvenation of the crystal mush accompanied by magma mixing and mingling. Based on zircon stability, the time required to heat, erupt and then cool to background conditions is relatively short, lasting a maximum of 10 s-1000 s years. Rejuvenation events in the LVC are ephemeral and permit eruption within an otherwise waning and cooling magmatic body.

Advances in containment methods and plutonium recovery strategies that led to the structural characterization of plutonium(IV) tetrachloride tris-diphenylsulfoxide, PuCl 4(OSPh 2) 3

DOE PAGES

Schrell, Samantha K.; Boland, Kevin Sean; Cross, Justin Neil; ...

2017-01-18

In an attempt to further advance the understanding of plutonium coordination chemistry, we report a robust method for recycling and obtaining plutonium aqueous stock solutions that can be used as a convenient starting material in plutonium synthesis. This approach was used to prepare and characterize plutonium(IV) tetrachloride tris-diphenylsulfoxide, PuCl 4(OSPh 2) 3, by single crystal X-ray diffraction. The PuCl 4(OSPh 2) 3 compound represents a rare example of a 7-coordinate plutonium(IV) complex. Structural characterization of PuCl 4(OSPh 2) 3 by X-ray diffraction utilized a new containment method for radioactive crystals. The procedure makes use of epoxy, polyimide loops, and amore » polyester sheath to provide a robust method for safely containing and easily handling radioactive samples. Lastly, the described procedure is more user friendly than traditional containment methods that employ fragile quartz capillary tubes. Additionally, moving to polyester, instead of quartz, lowers the background scattering from the heavier silicon atoms.« less

Negative refraction in one- and two-dimensional lossless plasma dielectric photonic crystals

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

Guo, B.

2013-07-15

Negative refraction in one- and two-dimensional lossless plasma dielectric photonic crystals consisting of plasma and background materials is theoretically investigated and the necessary conditions for negative refraction in these two structures are obtained. The critical frequency ω{sub 0} and the bandwidth Δω for negative refraction are explored, and the parameter dependence of effects such as plasma filling factor and the dielectric constant of background materials is also examined and discussed.

Practical physics behind growing crystals of biological macromolecules.

PubMed

Candoni, Nadine; Grossier, Romain; Hammadi, Zoubida; Morin, Roger; Veesler, Stéphane

2012-07-01

The aim of this review is to provide biocrystallographers who intend to tackle protein-crystallization with theory and practical examples. Crystallization involves two separate processes, nucleation and growth, which are rarely completely unconnected. Here we give theoretical background and concrete examples illustrating protein crystallization. We describe the nucleation of a new phase, solid or liquid, and the growth and transformation of existing crystals obtained by primary or secondary nucleation or by seeding. Above all, we believe that a thorough knowledge of the phase diagram is vital to the selection of starting position and path for any crystallization experiment.

Spatially selective photonic crystal enhanced fluorescence and application to background reduction for biomolecule detection assays

PubMed Central

Chaudhery, Vikram; Huang, Cheng-Sheng; Pokhriyal, Anusha; Polans, James; Cunningham, Brian T.

2011-01-01

By combining photonic crystal label-free biosensor imaging with photonic crystal enhanced fluorescence, it is possible to selectively enhance the fluorescence emission from regions of the PC surface based upon the density of immobilized capture molecules. A label-free image of the capture molecules enables determination of optimal coupling conditions of the laser used for fluorescence imaging of the photonic crystal surface on a pixel-by-pixel basis, allowing maximization of fluorescence enhancement factor from regions incorporating a biomolecule capture spot and minimization of background autofluorescence from areas between capture spots. This capability significantly improves the contrast of enhanced fluorescent images, and when applied to an antibody protein microarray, provides a substantial advantage over conventional fluorescence microscopy. Using the new approach, we demonstrate detection limits as low as 0.97 pg/ml for a representative protein biomarker in buffer. PMID:22109210

Spatially selective photonic crystal enhanced fluorescence and application to background reduction for biomolecule detection assays.

PubMed

Chaudhery, Vikram; Huang, Cheng-Sheng; Pokhriyal, Anusha; Polans, James; Cunningham, Brian T

2011-11-07

By combining photonic crystal label-free biosensor imaging with photonic crystal enhanced fluorescence, it is possible to selectively enhance the fluorescence emission from regions of the PC surface based upon the density of immobilized capture molecules. A label-free image of the capture molecules enables determination of optimal coupling conditions of the laser used for fluorescence imaging of the photonic crystal surface on a pixel-by-pixel basis, allowing maximization of fluorescence enhancement factor from regions incorporating a biomolecule capture spot and minimization of background autofluorescence from areas between capture spots. This capability significantly improves the contrast of enhanced fluorescent images, and when applied to an antibody protein microarray, provides a substantial advantage over conventional fluorescence microscopy. Using the new approach, we demonstrate detection limits as low as 0.97 pg/ml for a representative protein biomarker in buffer.

Survival condition for low-frequency quasi-one-dimensional breathers in a two-dimensional strongly anisotropic crystal

NASA Astrophysics Data System (ADS)

Savin, A. V.; Zubova, E. A.; Manevitch, L. I.

2005-06-01

We investigate a two-dimensional (2D) strongly anisotropic crystal (2D SAC) on substrate: 2D system of coupled linear chains of particles with strong intrachain and weak interchain interactions, each chain being subjected to the sine background potential. Nonlinear dynamics of one of these chains when the rest of them are fixed is reduced to the well known Frenkel-Kontorova (FK) model. Depending on strengh of the substrate, the 2D SAC models a variety of physical systems: polymer crystals with identical chains having light side groups, an array of inductively coupled long Josephson junctions, anisotropic crystals having light and heavy sublattices. Continuum limit of the FK model, the sine-Gordon (sG) equation, allows two types of soliton solutions: topological solitons and breathers. It is known that the quasi-one-dimensional topological solitons can propagate also in a chain of 2D system of coupled chains and even in a helix chain in a three-dimensional model of polymer crystal. In contrast to this, numerical simulation shows that the long-living breathers inherent to the FK model do not exist in the 2D SAC with weak background potential. The effect changes scenario of kink-antikink collision with small relative velocity: at weak background potential the collision always results only in intensive phonon radiation while kink-antikink recombination in the FK model results in long-living low-frequency sG breather creation. We found the survival condition for breathers in the 2D SAC on substrate depending on breather frequency and strength of the background potential. The survival condition bears no relation to resonances between breather frequency and frequencies of phonon band—contrary to the case of the FK model.

Fourier transform-infrared studies of thin H2SO4/H2O films: Formation, water uptake, and solid-liquid phase changes

NASA Technical Reports Server (NTRS)

Middlebrook, Ann M.; Iraci, Laura T.; Mcneill, Laurie S.; Koehler, Birgit G.; Wilson, Margaret A.; Saastad, Ole W.; Tolbert, Margaret A.; Hanson, David R.

1993-01-01

Fourier transform-infrared (FTIR) spectroscopy was used to examine films representative of stratospheric sulfuric acid aerosols. Thin films of sulfuric acid were formed in situ by the condensed phase reaction of SO3 with H2O. FTIR spectra show that the sulfuric acid films absorb water while cooling in the presence of water vapor. Using stratospheric water pressures, the most dilute solutions observed were greater than 40 wt % before simultaneous ice formation and sulfuric acid freezing occurred. FTIR spectra also revealed that the sulfuric acid films crystallized mainly as sulfuric acid tetrahydrate (SAT). Crystallization occurred either when the composition was about 60 wt% H2SO4 or after ice formed on the films at temperatures 1-4 K below the ice frost point. Finally, we determined that the melting point for SAT depended on the background water pressure and was 216-219 K in the presence of 4 x 10(exp -4) Torr H2O. Our results suggest that once frozen, sulfuric acid aerosols in the stratosphere are likely to melt at these temperatures, 30 K colder than previously thought.

A Program of Research on Microfabrication Techniques for VLSI Magnetic Devices.

DTIC Science & Technology

1982-10-01

contribution to the implantation- induced uniaxial anisotropy field change. BACKGROUND Magnetic garnet films are grown by liquid phase epitaxy ( LPE ) on non...a single crystal, non-magnetic garnet substrate by the liquid phase epitaxy ( LPE ) method. These thin films , usually one to three microns in thickness...microscopy. Experimental Procedures Films of (SmYGdTm)3Ca0a.Fe4.6012 garnet were grown by liquid phase epitaxy ( LPE ) on gadolinium-gallium garnet (GGG

The DARPA High-Performance Polymer Program. Volume 1. Program Background and Highlights of the Program Review Held on 14-15 January 1992

DTIC Science & Technology

1992-09-01

conducting polyaniline for military systems is extensive and ranges from lightning-strike protection to utilization in honeycomb structures in aircraft...Conducting polyanilines are representative of a new class of materials known as synthetic metals. This technology is still discovering new and varied...metals using polyaniline chemistry 2" High-definition liquid crystal displays 3 Polymeric piezoelectric materials 4 Drag-reducing polymers for ship

Phonons in a magnetized Coulomb crystal of ions with polarizable electron background

NASA Astrophysics Data System (ADS)

Baiko, D. A.; Kozhberov, A. A.

2017-11-01

We have studied phonon modes of a body-centered cubic (bcc) Coulomb crystal of ions in the presence of a uniform magnetic field B taking into account the polarizability of the electron background (electron screening) described by the Thomas-Fermi formalism. For k ≫κTF (k and κTF are the phonon wavevector and Thomas-Fermi wavenumber, respectively), electron polarizability is not important. At k ≪κTF , the electron response results in a pronounced effect. One of the three available modes is acoustic. For orthogonal propagation ( k ⊥B ), its frequency Ω is independent of B and κTF . For k ∥B , Ω∝1 /κTF and is independent of B. Another mode is quadratic. Its frequency is ∝1 /(B κTF) for orthogonal propagation and ∝1 /B and independent of κTF for the parallel case. The third mode is optic with Ω≈ωB ( ωB is the ion cyclotron frequency). A general expression is derived for the dynamic matrix of a Coulomb crystal with a polarizable background and more than one ion in the primitive cell. It is employed for a study of a magnetized hexagonal close-packed Coulomb crystal. We have also presented an analysis of phonon polarization vectors in a magnetized bcc crystal with or without screening. The results obtained can be used for realistic calculations of electron-phonon scattering rates and electron thermal and electrical conductivities in neutron star crusts.

Coulomb crystals in neutron star crust

NASA Astrophysics Data System (ADS)

Baiko, D. A.

2014-03-01

It is well known that neutron star crust in a wide range of mass densities and temperatures is in a crystal state. At a given density, the crystal is made of fully ionized atomic nuclei of a single species immersed in a nearly incompressible (i.e., constant and uniform) charge compensating background of electrons. This model is known as the Coulomb crystal model. In this talk we analyze thermodynamic and elastic properties of the Coulomb crystals and discuss various deviations from the ideal model. In particular, we study the Coulomb crystal behavior in the presence of a strong magnetic field, consider the effect of the electron gas polarizability, outline the main properties of binary Coulomb crystals, and touch the subject of quasi-free neutrons permeating the Coulomb crystal of ions in deeper layers of neutron star crust.

EAST WALL OF CRYSTALLIZER WING TO THE LEFT, END WALL ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

EAST WALL OF CRYSTALLIZER WING TO THE LEFT, END WALL OF CRUSHING MILL IN CENTER. GABLE END OF BOILING HOUSE IN LEFT BACKGROUND. VIEW FROM THE SOUTH - Kekaha Sugar Company, Sugar Mill Building, 8315 Kekaha Road, Kekaha, Kauai County, HI

Search for solar axions

NASA Astrophysics Data System (ADS)

Newman, Seth Aaron

Peccei and Quinn proposed an elegant solution for restoring CP symmetry to the QCD Lagrangian [37]. This method includes an additional global U(1) symmetry included in the QCD Lagrangian which is spontaneously broken at a high energy scale, fa. Breaking the symmetry generates a Nambu-Goldstone boson called the axion. Although there are various detection mechanisms that search for the axion, this thesis focuses on the the axio-electric effect. The axio-electric is similar to the photo-electric effect in that an axion is absorbed by an atom which subsequently emits an electron. The electron's energy is equivalent to the incoming axion energy minus the binding energy. The higher shell electrons immediately replenish the missing binding energy yielding a single energy peak at the incoming axion's energy. The 14.4 keV M1 transition of 57Fe is one possible axion source. The development of an optimum trigger algorithm has lowered the threshold for analysis in TeO2 bolometers to a few keV making an axion signature accessible to CUORE related R&D experiments such as the Chinese Crystal Validation Runs (CCVR) and Three Towers Test (TTT). These TeO2 crystal detectors have masses 750 and 790 grams, respectively. Each crystal has a stabilization heater and a germanium thermometer attached to its surface by an epoxy glue. The two previous experiments are R&D tests for the upcoming larger experiment, CUORE. CUORE will be made of 988 TeO2 crystals arranged in 19 towers with 13 floors each, each floor with 4 detectors. This thesis examined 87.01 kg·days of Three Towers data for an axion signal. A peak is observed in the region of interest with a statistical significance less than 1sigma over the expected background fluctuations, yielding a total background rate of 0.185 +/- 0.001 (Stat.) +/- 0.006 (Syst.) Counts/kg/day at 95% C.L. This places an experimental limit on the coupling constant fa of f a (S = 0.50) ≥ 1.16 x 106 GeV at 95% C.L. Projecting the TTT result to the CUORE mass and a five year run time we can expect a limit of fa(S = 0.50) ≥ 2.21 x 106 GeV at 95% C.L. Improvements in granularity can strengthen the bound on fa by 8% and 25% for background reductions by a factor of 2 and 10, respectively.

The LUCIFER Project: Achievements and Near Future Prospects

NASA Astrophysics Data System (ADS)

Beeman, J. W.; Bellini, F.; Benetti, P.; Cardani, L.; Casali, N.; Chiesa, D.; Clemenza, M.; Dafinei, I.; Di Domizio, S.; Ferroni, F.; Gironi, L.; Giuliani, A.; Gotti, C.; Maino, M.; Nagorny, S. S.; Nisi, S.; Nones, C.; Pagnanini, L.; Pattavina, L.; Pessina, G.; Piperno, G.; Pirro, S.; Previtali, E.; Rusconi, C.; Schäffner, K.; Tomei, C.; Vignati, M.

2016-08-01

In the view of exploring the inverted hierarchy region future experiments investigating the neutrinoless double beta decay have to demand for detectors with excellent energy resolution and zero background in the energy region of interest. Cryogenic scintillating bolometers are very suitable detectors for this task since they provide particle discrimination: the simultaneous detection of the phonon and light signal allows us to identify the interacting type of particle and thus guarantees a suppression of α -induced backgrounds, the key-issue for next-generation tonne-scale bolometric experiments. The LUCIFER project aims at running the first array of enriched scintillating Zn^{ {82}}Se bolometers (total mass of about 8kg of ^{ {82}}Se) with a background level as low as 10^{ {-3}} counts/(keV kg y) in the energy region of interest. The main effort is currently focused on the finalization of the crystal growth procedure in order to achieve high quality Zn^{ {82}}Se crystals both in terms of radiopurity and bolometric properties. We present results from tests of such crystals operated at mK temperatures which demonstrate the excellent background rejection capabilities of this detection approach towards a background-free demonstrator experiment. Besides, the high purity of the enriched ^{ {82}}Se material allows us to establish the most stringent limits on the half-life of the double beta decay of ^{ {82}}Se on excited levels.

Localized Rejuvenation of a Crystal Mush Recorded in Zircon Temporal and Compositional Variation at the Lassen Volcanic Center, Northern California

PubMed Central

Klemetti, Erik W.; Clynne, Michael A.

2014-01-01

Zircon ages and trace element compositions from recent silicic eruptions in the Lassen Volcanic Center (LVC) allow for an evaluation of the timing and conditions of rejuvenation (reheating and mobilization of crystals) within the LVC magmatic system. The LVC is the southernmost active Cascade volcano and, prior to the 1980 eruption of Mount St. Helens, was the site of the only eruption in the Cascade arc during the last century. The three most recent silicic eruptions from the LVC were very small to moderate-sized lava flows and domes of dacite (1915 and 27 ka eruptions of Lassen Peak) and rhyodacite (1.1 ka eruption of Chaos Crags). These eruptions produced mixed and mingled lavas that contain a diverse crystal cargo, including zircon. 238U-230Th model ages from interior and surface analyses of zircon reveal ages from ∼17 ka to secular equilibrium (>350 ka), with most zircon crystallizing during a period between ∼60–200 ka. These data support a model for localized rejuvenation of crystal mush beneath the LVC. This crystal mush evidently is the remnant of magmatism that ended ∼190 ka. Most zircon are thought to have been captured from “cold storage” in the crystal mush (670–725°C, Hf >10,000 ppm, Eu/Eu* 0.25–0.4) locally remobilized by intrusion of mafic magma. A smaller population of zircon (>730°C, Hf <10,000 ppm, Eu/Eu* >0.4) grew in, and are captured from, rejuvenation zones. These data suggest the dominant method to produce eruptible melt within the LVC is small-scale, local rejuvenation of the crystal mush accompanied by magma mixing and mingling. Based on zircon stability, the time required to heat, erupt and then cool to background conditions is relatively short, lasting a maximum of 10 s–1000 s years. Rejuvenation events in the LVC are ephemeral and permit eruption within an otherwise waning and cooling magmatic body. PMID:25470726

Spherical quartz crystals investigated with synchrotron radiation

DOE PAGES

Pereira, N. R.; Macrander, A. T.; Hill, K. W.; ...

2015-10-27

The quality of x-ray spectra and images obtained from plasmas with spherically bent crystals depends in part on the crystal's x-ray diffraction across the entire crystal surface. We employ the energy selectivity and high intensity of synchrotron radiation to examine typical spherical crystals from alpha-quartz for their diffraction quality, in a perpendicular geometry that is particularly convenient to examine sagittal focusing. The crystal's local diffraction is not ideal: the most noticeable problems come from isolated regions that so far have failed to correlate with visible imperfections. In conclusion, excluding diffraction from such problem spots has little effect on the focusmore » beyond a decrease in background.« less

Development of CDMS-II Surface Event Rejection Techniques and Their Extensions to Lower Energy Thresholds

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

Hofer, Thomas James

2014-12-01

The CDMS-II phase of the Cryogenic Dark Matter Search, a dark matter direct-detection experiment, was operated at the Soudan Underground Laboratory from 2003 to 2008. The full payload consisted of 30 ZIP detectors, totaling approximately 1.1 kg of Si and 4.8 kg of Ge, operated at temperatures of 50 mK. The ZIP detectors read out both ionization and phonon pulses from scatters within the crystals; channel segmentation and analysis of pulse timing parameters allowed e ective ducialization of the crystal volumes and background rejection su cient to set world-leading limits at the times of their publications. A full re-analysis ofmore » the CDMS-II data was motivated by an improvement in the event reconstruction algorithms which improved the resolution of ionization energy and timing information. The Ge data were re-analyzed using three distinct background-rejection techniques; the Si data from runs 125 - 128 were analyzed for the rst time using the most successful of the techniques from the Ge re-analysis. The results of these analyses prompted a novel \\mid-threshold" analysis, wherein energy thresholds were lowered but background rejection using phonon timing information was still maintained. This technique proved to have signi cant discrimination power, maintaining adequate signal acceptance and minimizing background leakage. The primary background for CDMS-II analyses comes from surface events, whose poor ionization collection make them di cult to distinguish from true nuclear recoil events. The novel detector technology of SuperCDMS, the successor to CDMS-II, uses interleaved electrodes to achieve full ionization collection for events occurring at the top and bottom detector surfaces. This, along with dual-sided ionization and phonon instrumentation, allows for excellent ducialization and relegates the surface-event rejection techniques of CDMS-II to a secondary level of background discrimination. Current and future SuperCDMS results hold great promise for mid- to low-mass WIMP-search results.« less

Crystal engineering: co-crystals of cinnamic acid derivatives with a pyridyl derivative co-crystallizer.

PubMed

Lorenzo, Daniel A; Forrest, Sebastian J K; Sparkes, Hazel A

2016-02-01

A number of hydrogen-bonded co-crystals, consisting of a cinnamic acid derivative and a pyridyl co-crystallizer, have been synthesized and their properties investigated by X-ray diffraction. Samples were prepared by recrystallization or solvent drop grinding of trans-cinnamic acid (1), 4-methylcinnamic acid (2), 4-methoxy cinnamic acid (3) or 3,4-methoxy cinnamic acid (4), with 4,4-dipyridyl (A), iso-nicotinamide (B) or nicotinamide (C). The X-ray single-crystal structures of seven novel co-crystals, obtained through recrystallization, are examined and the hydrogen-bonding interactions discussed. Consistent hydrogen-bonding motifs were observed for samples prepared when using 4,4-dipyridyl (A) or iso-nicotinamide (B) as the co-crystallizing agent. Powder X-ray diffraction analysis of the samples prepared by solvent drop grinding suggests the formation of ten co-crystals.

Top-seeded solution growth and morphology change of RbTiOPO4:Ta single crystal

NASA Astrophysics Data System (ADS)

Li, Ziqing; Chen, Yang; Zhu, Pengfei; Ji, Nianjing; Duan, Xiulan; Jiang, Huaidong

2018-04-01

The RbTiOPO4:Ta single crystal with dimensions of 4 mm × 31 mm × 18 mm was successfully grown by Top Seeded Solution Growth Technique. It is concluded that the doping Ta element can strongly influence the growth and morphology of the RbTiOPO4 crystal. The evident morphology change of RbTiOPO4:Ta crystal with respect to RbTiOPO4 crystal has been observed and the (1 0 0) crystal face was more developed than any other crystal faces. The possible reasons of the morphology change were analyzed through experimental and theoretical methods. Several methods were tried to increase crystallographic a direction dimension of RbTiOPO4:Ta crystals. Finally, the RbTiOPO4:Ta single crystal with crystallographic a direction dimension up to 6 mm was obtained by using thicker seed crystal. This way makes it possible to get isometric RbTiOPO4:Ta crystals, which is beneficial for nonlinear optical applications due to larger area in x-y plane.

STS study on single crystal of noncentrosymmetric superconductor PbTaSe2

NASA Astrophysics Data System (ADS)

Ye, Zhiyang; Wu, Rui; Wang, Jihui; Liang, Xuejin; Mao, Hanqing; Zhao, Lingxiao; Chen, Genfu; Pan, Shuheng

2015-03-01

We report our low temperature scanning tunneling spectroscopic study on single crystals of noncentrosymmetric superconductor PbTaSe2. On the background of the normal state tunneling spectrum, a superconducting energy gap opens at a temperature below the bulk Tc = 3.7K. At t = 1.4K, the gap magnitude is estimated to be about 1meV. This energy gap is particle-hole symmetry and is homogeneous in space. Extrapolating the low energy part of the spectrum, we find that the low energy part of the gap spectrum is linear like ``V'' shape. We will present the results of the numerical fit with various gap functions of proposed possible pairing symmetry. We will also present our preliminary results of the magnetic field dependence measurement and discuss the implications of these observations.

Single crystalline Co3O4 nanocrystals exposed with different crystal planes for Li-O2 batteries.

PubMed

Su, Dawei; Dou, Shixue; Wang, Guoxiu

2014-08-29

Single crystalline Co3O4 nanocrystals exposed with different crystal planes were synthesised, including cubic Co3O4 nanocrystals enclosed by {100} crystal planes, pseudo octahedral Co3O4 enclosed by {100} and {110} crystal planes, Co3O4 nanosheets exposed by {110} crystal planes, hexagonal Co3O4 nanoplatelets exposed with {111} crystal planes, and Co3O4 nanolaminar exposed with {112} crystal planes. Well single crystalline features of these Co3O4 nanocrystals were confirmed by FESEM and HRTEM analyses. The electrochemical performance for Li-O2 batteries shows that Co3O4 nanocrystals can significantly reduce the discharge-charge over-potential via the effect on the oxygen evolution reaction (OER). From the comparison on their catalytic performances, we found that the essential factor to promote the oxygen evolution reactions is the surface crystal planes of Co3O4 nanocrystals, namely, crystal planes-dependent process. The correlation between different Co3O4 crystal planes and their effect on reducing charge-discharge over-potential was established: {100} < {110} < {112} < {111}.

Resolution Enhancement in PET Reconstruction Using Collimation

NASA Astrophysics Data System (ADS)

Metzler, Scott D.; Matej, Samuel; Karp, Joel S.

2013-02-01

Collimation can improve both the spatial resolution and sampling properties compared to the same scanner without collimation. Spatial resolution improves because each original crystal can be conceptually split into two (i.e., doubling the number of in-plane crystals) by masking half the crystal with a high-density attenuator (e.g., tungsten); this reduces coincidence efficiency by 4× since both crystals comprising the line of response (LOR) are masked, but yields 4× as many resolution-enhanced (RE) LORs. All the new RE LORs can be measured by scanning with the collimator in different configurations.In this simulation study, the collimator was assumed to be ideal, neither allowing gamma penetration nor truncating the field of view. Comparisons were made in 2D between an uncollimated small-animal system with 2-mm crystals that were assumed to be perfectly absorbing and the same system with collimation that narrowed the effective crystal size to 1 mm. Digital phantoms included a hot-rod and a single-hot-spot, both in a uniform background with activity ratio of 4:1. In addition to the collimated and uncollimated configurations, angular and spatial wobbling acquisitions of the 2-mm case were also simulated. Similarly, configurations with different combinations of the RE LORs were considered including (i) all LORs, (ii) only those parallel to the 2-mm LORs; and (iii) only cross pairs that are not parallel to the 2-mm LORs. Lastly, quantitative studies were conducted for collimated and uncollimated data using contrast recovery coefficient and mean-squared error (MSE) as metrics. The reconstructions show that for most noise levels there is a substantial improvement in image quality (i.e., visual quality, resolution, and a reduction in artifacts) by using collimation even when there are 4 fewer counts or-in some cases-comparing with the noiseless uncollimated reconstruction. By comparing various configurations of sampling, the results show that it is the matched combination of both improved spatial resolution of each LOR and the increase in the number of LORs that yields improved reconstructions. Further, the quantitative studies show that for low-count scans, the collimated data give better MSE for small lesions and the uncollimated data give better MSE for larger lesions; for highcount studies, the collimated data yield better quantitative values for the entire range of lesion sizes that were evaluated.

Molarity (Aromic Density) of the Elements as Pure Crystals.

ERIC Educational Resources Information Center

Pauling, Linus; Herman, Zelek S.

1985-01-01

Provides background information for teachers on the atomic density of the elements as pure crystals. Atomic density is defined as the reciprocal of the atomic volume. Includes atomic-density diagrams which were prepared using the atomic-volume values given by Singman, supplemented by additional values for some allotropes. (JN)

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.

The improved scintillation crystal lead tungstate scintillation for PET

NASA Astrophysics Data System (ADS)

Wan, Youbao; WU, Rurong; Xiao, Linrong; Zhang, Jianxin; Yang, Peizhi; Yan, Hui

2009-07-01

As a valuable material for the detecting of γ-ray, PbWO4 and BaF2:PbWO4 crystals were grown by a novel multi-crucible temperature gradient system developed by ourselves. Utilizing a topical partial heating method, this system can form a topical partial high temperature in its hearth. Thus this system could melt raw materials in step by step as requirement. The advantage of this method is that there would be solid obstruct left on the melt in the procedure of the crystal growing up. The left obstruct could prevent the volatilization of the component in the melt. Hence it is helpful for the composition homogenization in the crystal. The system also offers a sustaining device for multi-crucibles and thus it can grow many crystals simultaneity. The optical properties and scintillation properties of the crystals were studied. The results reveal that the ions doping improves the scintillation properties of the crystal. The transmittance spectra show that the transmittance of BaF2:PbWO4 crystals are better than that of PbWO4 crystals. For the PbWO4 crystals, their absorption edge is at 325nm, and their maximum transmittance is 68%. For the BaF2:PbWO4 crystals, their absorption edge is at 325nm and their maximum transmittance is upto76%. The X-ray excited luminescence spectra shows that the luminescence peak is at 420nm for the samples of PbWO4 crystal while the peak is at 430nm for the samples of BaF2:PbWO4 crystal respectively. The luminescence intensity of the samples of BaF2:PbWO4 crystal is about two times than that of PbWO4 crystal. And their peak shape is different for the two kind of crystal. The light yield of BaF2:PbWO4 crystals is about 2.9 times than that of PbWO4 crystal Analyzing these scintillation properties, we find that the VPb 3+ and VO- defects do harm for the optical properties of the crystal. Ions doping method could reduce the defect concentration and improving its illumination performance of the crystal. Specially, the doped F- ions in O2- site can induce the aberrance of the [WO4]2- tetrahedron and form [WO3F]- tetrahedron which has more active blue light yield, thus improve the light yield of the crystal. The improved light yield of BaF2:PbWO4 crystals is valuable for the medical diagnosing instrument PET and CT with high resolving power

Coupling effects for separate spatial solitons in a biased series centrosymmetric photorefractive crystal circuit considering grey solitons

NASA Astrophysics Data System (ADS)

Katti, Aavishkar; Yadav, Ram Anjore

2018-02-01

The existence and coupling of grey-grey, grey-bright and grey-dark separate spatial solitons in a biased series centrosymmetric photorefractive crystal circuit is investigated for the first time. The numerical solution of the separate spatial solitons is presented. The coupling between the two separate spatial solitons is analysed for all three cases of separate coupled solitons, namely grey-grey, grey-bright, and grey-dark. Changing the intensity of the soliton in one crystal affects the soliton in both crystals due to flow of the light induced current through the circuit. The effect of the background intensity of each crystal on both the spatial solitons is investigated. Also, the effect of changing the temperature of one crystal affects the soliton in both crystals due to the coupling effect. The soliton width dependence on the temperature is different for each crystal.

Single Crystalline Co3O4 Nanocrystals Exposed with Different Crystal Planes for Li-O2 Batteries

PubMed Central

Su, Dawei; Dou, Shixue; Wang, Guoxiu

2014-01-01

Single crystalline Co3O4 nanocrystals exposed with different crystal planes were synthesised, including cubic Co3O4 nanocrystals enclosed by {100} crystal planes, pseudo octahedral Co3O4 enclosed by {100} and {110} crystal planes, Co3O4 nanosheets exposed by {110} crystal planes, hexagonal Co3O4 nanoplatelets exposed with {111} crystal planes, and Co3O4 nanolaminar exposed with {112} crystal planes. Well single crystalline features of these Co3O4 nanocrystals were confirmed by FESEM and HRTEM analyses. The electrochemical performance for Li-O2 batteries shows that Co3O4 nanocrystals can significantly reduce the discharge-charge over-potential via the effect on the oxygen evolution reaction (OER). From the comparison on their catalytic performances, we found that the essential factor to promote the oxygen evolution reactions is the surface crystal planes of Co3O4 nanocrystals, namely, crystal planes-dependent process. The correlation between different Co3O4 crystal planes and their effect on reducing charge-discharge over-potential was established: {100} < {110} < {112} < {111}. PMID:25169737

Low-temperature relative reflectivity measurements of reflective and scintillating foils used in rare event searches

NASA Astrophysics Data System (ADS)

Langenkämper, A.; Ulrich, A.; Defay, X.; Feilitzsch, F. v.; Lanfranchi, J.-C.; Mondragón, E.; Münster, A.; Oppenheimer, C.; Potzel, W.; Roth, S.; Schönert, S.; Steiger, H.; Trinh Thi, H. H.; Wawoczny, S.; Willers, M.; Zöller, A.

2018-03-01

In this work we investigate the reflectivity of highly reflective multilayer polymer foils used in the CRESST experiment. The CRESST experiment searches directly for dark matter via operating scintillating CaWO4 crystals as targets for elastic dark matter-nucleon scattering. In order to suppress background events, the experiment employs the so-called phonon-light technique which is based on the simultaneous measurement of the heat signal in the main CaWO4 target crystal and of the emitted scintillation light with a separate cryogenic light detector. Both detectors are surrounded by a highly reflective and scintillating multilayer polymer foil to increase the light collection efficiency and to veto surface backgrounds. While this study is motivated by the CRESST experiment, the results are also relevant for other rare event searches using scintillating cryogenic bolometers in the field of the search of dark matter and neutrinoless double beta decay (0 νββ). In this work a dedicated experiment has been set up to determine the relative reflectivity at 300 K and 20 K of three multilayer foils ("VM2000", "VM2002", "Vikuiti") produced by the company 3M. The intensity of a light beam reflected off the foil is measured with a CCD camera. The ratio of the intensities at 300 K and 20 K corresponds to the relative reflectivity change. The measurements performed in this work show no variation of the reflectivity with temperature at a level of ∼1%.

Additional evidence from x-ray powder diffraction patterns that icosahedral quasi-crystals of intermetallic compounds are twinned cubic crystals

PubMed Central

Pauling, Linus

1988-01-01

Analysis of the measured values of Q for the weak peaks (small maxima, usually considered to be background fluctuations, “noise”) on the x-ray powder diffraction curves for 17 rapidly quenched alloys leads directly to the conclusion that they are formed by an 820-atom or 1012-atom primitive cubic structure that by icosahedral twinning produces the so-called icosahedral quasi-crystals. PMID:16593948

Synthesis, growth, structural, optical and thermal properties of an organic single crystal: 4-nitroaniline 4-aminobenzoic acid.

PubMed

Silambarasan, A; Rajesh, P; Ramasamy, P

2014-01-24

The organic single crystals of 4-nitroaniline 4-aminobenzoic acid (4NAABA) were grown from ethanol solvent. The lattice parameters of the grown crystal have been confirmed from single crystal XRD analysis. The powder XRD pattern shows the various planes of grown crystal. The FTIR and (1)H NMR spectral analysis confirm the presence of various functional groups and the placement of proton in 4NAABA compound respectively. The UV absorption was carried out which shows the cutoff wavelength around 459 nm. The optical band gap of the crystal has been evaluated from the transmission spectra and absorption coefficient by extrapolation technique. In addition, a fluorescence spectral analysis is carried out for 4NAABA crystals. The thermal properties of crystals were evaluated from thermogravimetrical analysis. It shows that the grown crystal is stable up to 160°C and the crystal has sharp melting point at 151°C. Copyright © 2013 Elsevier B.V. All rights reserved.

A graphite crystal polarimeter for stellar X-ray astronomy.

NASA Technical Reports Server (NTRS)

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

1972-01-01

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

Activity-induced instability of phonons in 1D microfluidic crystals.

PubMed

Tsang, Alan Cheng Hou; Shelley, Michael J; Kanso, Eva

2018-02-14

One-dimensional crystals of passively-driven particles in microfluidic channels exhibit collective vibrational modes reminiscent of acoustic 'phonons'. These phonons are induced by the long-range hydrodynamic interactions among the particles and are neutrally stable at the linear level. Here, we analyze the effect of particle activity - self-propulsion - on the emergence and stability of these phonons. We show that the direction of wave propagation in active crystals is sensitive to the intensity of the background flow. We also show that activity couples, at the linear level, transverse waves to the particles' rotational motion, inducing a new mode of instability that persists in the limit of large background flow, or, equivalently, vanishingly small activity. We then report a new phenomenon of phonons switching back and forth between two adjacent crystals in both passively-driven and active systems, similar in nature to the wave switching observed in quantum mechanics, optical communication, and density stratified fluids. These findings could have implications for the design of commercial microfluidic systems and the self-assembly of passive and active micro-particles into one-dimensional structures.

Synthesis, crystal growth, structural, thermal, optical and mechanical properties of solution grown 4-methylpyridinium 4-hydroxybenzoate single crystal.

PubMed

Sudhahar, S; Krishna Kumar, M; Sornamurthy, B M; Mohan Kumar, R

2014-01-24

Organic nonlinear optical material, 4-methylpyridinium 4-hydroxybenzoate (4MPHB) was synthesized and single crystal was grown by slow evaporation solution growth method. Single crystal and powder X-ray diffraction analyses confirm the structure and crystalline perfection of 4MPHB crystal. Infrared, Raman and NMR spectroscopy techniques were used to elucidate the functional groups present in the compound. TG-DTA analysis was carried out in nitrogen atmosphere to study the decomposition stages, endothermic and exothermic reactions. UV-visible and Photoluminescence spectra were recorded for the grown crystal to estimate the transmittance and band gap energy respectively. Linear refractive index, birefringence, and SHG efficiency of the grown crystal were studied. Laser induced surface damage threshold and mechanical properties of grown crystal were studied to assess the suitability of the grown crystals for device applications. Copyright © 2013 Elsevier B.V. All rights reserved.

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography.

PubMed

Gicquel, Yannig; Schubert, Robin; Kapis, Svetlana; Bourenkov, Gleb; Schneider, Thomas; Perbandt, Markus; Betzel, Christian; Chapman, Henry N; Heymann, Michael

2018-04-24

This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The devices are patterned from epoxy glue using soft lithography and are suitable for in situ X-ray diffraction experiments at room temperature. The sample wells are lidded on both sides with polymeric polyimide foil windows that allow diffraction data collection with low X-ray background. This fabrication method is undemanding and inexpensive. After the sourcing of a SU-8 master wafer, all fabrication can be completed outside of a cleanroom in a typical research lab environment. The chip design and fabrication protocol utilize capillary valving to microfluidically split an aqueous reaction into defined nanoliter sized droplets. This loading mechanism avoids the sample loss from channel dead-volume and can easily be performed manually without using pumps or other equipment for fluid actuation. We describe how isolated nanoliter sized drops of protein solution can be monitored in situ by dynamic light scattering to control protein crystal nucleation and growth. After suitable crystals are grown, complete X-ray diffraction datasets can be collected using goniometer based in situ fixed target serial X-ray crystallography at room temperature. The protocol provides custom scripts to process diffraction datasets using a suite of software tools to solve and refine the protein crystal structure. This approach avoids the artefacts possibly induced during cryo-preservation or manual crystal handling in conventional crystallography experiments. We present and compare three protein structures that were solved using small crystals with dimensions of approximately 10-20 µm grown in chip. By crystallizing and diffracting in situ, handling and hence mechanical disturbances of fragile crystals is minimized. The protocol details how to fabricate a custom X-ray transparent microfluidic chip suitable for in situ serial crystallography. As almost every crystal can be used for diffraction data collection, these microfluidic chips are a very efficient crystal delivery method.

Buried chloride stereochemistry in the Protein Data Bank

PubMed Central

2014-01-01

Background Despite the chloride anion is involved in fundamental biological processes, its interactions with proteins are little known. In particular, we lack a systematic survey of its coordination spheres. Results The analysis of a non-redundant set (pairwise sequence identity?

From Mild to WildLV14378 Fluctuations in Crystal Plasticity

NASA Astrophysics Data System (ADS)

Weiss, J.; Rhouma, W. Ben; Richeton, T.; Dechanel, S.; Louchet, F.; Truskinovsky, L.

2015-03-01

Macroscopic crystal plasticity is classically viewed as an outcome of uncorrelated dislocation motions producing Gaussian fluctuations. An apparently conflicting picture emerged in recent years emphasizing highly correlated dislocation dynamics characterized by power-law distributed fluctuations. We use acoustic emission measurements in crystals with different symmetries to show that intermittent and continuous visions of plastic flow are not incompatible. We demonstrate the existence of crossover regimes where strongly intermittent events coexist with a Gaussian quasiequilibrium background and propose a simple theoretical framework compatible with these observations.

Cryomagnetic Point-Contact Andreev Reflection Spectroscopy on Single Crystal Iron-Chalcogenide Superconductors

NASA Astrophysics Data System (ADS)

Yen, Y. T.; Hu, Rongwei; Petrovic, C.; Yeh, K. W.; Wu, M. K.; Wei, J. Y. T.

2012-02-01

We report on cryomagnetic point-contact Andreev reflection spectroscopy performed on single crystals of superconducting FeTe1-xSx and FeTe1-xSex. The samples are cleaved in-situ and the measurements are carried out at temperatures down to 4.2K and in a field up to 9T. At base temperature and zero field, we observe a cone-shaped hump at lower voltages in the conductance spectra with no dips at zero bias and a linear background at higher voltages. The spectral evolution of gap size, zero-bias conductance, and excess spectral area are analyzed as a function of temperature and field. Further spectral analysis is carried out using theoretical models of conductance spectra in multiband superconductors [1,2] and of gap symmetry in Fe-based superconductors [3]. The role of interstitial iron is also considered, by comparison with atomically-resolved scanning tunneling spectroscopy data.[4pt] [1] V. Lukic and E.J. Nicol, PRB 76, 144508 (2007) [2] A. Golubov et al., PRL 103, 077003 (2009) [3] P.J. Hirschfeld et al., RPP 74, 124508 (2011)

Growth and characterization of benzyl 4-hydroxybenzoate single crystal by vertical Bridgman technique for optical applications

NASA Astrophysics Data System (ADS)

Solanki, S. Siva Bala; Rajesh, N. P.; Suthan, T.

2018-07-01

The benzyl 4-hydroxybenzoate single crystal has been grown by vertical Bridgman technique. The grown crystal was confirmed by single crystal X-ray diffraction studies. The presence of functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) spectral studies. The thermal behaviour of the grown crystal was analyzed by thermogravimetric analysis (TGA), differential thermal analysis (DTA) and differential scanning calorimetric (DSC) studies. Optical behaviour of the grown benzyl 4-hydroxybenzoate crystal was studied by UV-Vis-NIR spectral analysis. Fluorescence spectrum shows near violet light emission. The second harmonic generation behaviour of benzyl 4-hydroxybenzoate was analyzed. The laser damage threshold value of benzyl 4-hydroxybenzoate was measured as 2.16 GW/cm2. The dielectric measurements of benzyl 4-hydroxybenzoate crystal were carried out with different frequencies 1 kHz to 1 MHz versus different temperatures ranging from 313 to 353 K. Photoconductivity study shows that the grown benzyl 4-hydroxybenzoate crystal belongs to negative photoconductivity property. The mechanical strength of the crystal was calculated by Vickers microhardness study.

Physical chemistry of the H2SO4/HNO3/H2O system - Implications for polar stratospheric clouds

NASA Technical Reports Server (NTRS)

Molina, M. J.; Zhang, R.; Wooldridge, P. J.; Mcmahon, J. R.; Kim, J. E.; Chang, H. Y.; Beyer, K. D.

1993-01-01

Polar stratospheric clouds (PSCs) play a key role in stratospheric ozone depletion. Surface-catalyzed reactions on PSC particles generate chlorine compounds that photolyze readily to yield chlorine radicals, which in turn destroy ozone very efficiently. The most prevalent PSCs form at temperatures several degrees above the ice frost point and are believed to consist of HNO3 hydrates; however, their formation mechanism is unclear. Results of laboratory experiments are presented which indicate that the background stratospheric H2SO4/H2O aerosols provide an essential link in this mechanism: These liquid aerosols absorb significant amounts of HNO3 vapor, leading most likely to the crystallization of nitric acid trihydrate (NAT). The frozen particles then grow to form PSCs by condensation of additional amounts of HNO3 and H2O vapor. Furthermore, reaction probability measurements reveal that the chlorine radical precursors are formed readily at polar stratospheric temperatures not just on NAT and ice crystals, but also on liquid H2SO4 solutions and on solid H2SO4 hydrates. These results imply that the chlorine activation efficiency of the aerosol particles increases rapidly as the temperature approaches the ice frost point regardless of the phase or composition of the particles.

A cryogenic waveplate rotator for polarimetry at mm and submm wavelengths

NASA Astrophysics Data System (ADS)

Salatino, M.; de Bernardis, P.; Masi, S.

2011-04-01

Context. Polarimetry at mm and submm wavelengths is the new frontier of research in cosmic microwave background and interstellar dust studies. Polarimeters working in the IR to MM range need to be operated at cryogenic temperatures to limit the systematic effects related to the emission of the polarization analyzer. Aims: We study the effect of the temperature of the different components of a waveplate polarimeter and describe a system able to rotate a birefringent crystal at 4 K in a completely automated way. Methods: We simulate the main systematic effects related to the temperature and non-ideality of the optical components in a Stokes polarimeter. To limit these effects, a cryogenic implementation of the polarimeter is mandatory. In our system, the rotation produced by a step motor running at room temperature is transmitted down to cryogenic temperatures by means of a long shaft and gears running on custom cryogenic bearings. Results: Our system is able to rotate a birefringent crystal at 4 K in a completely automated way and dissipates only a few mW in the cold environment. A readout system based on optical fibers allows us to control the rotation of the crystal to better than 0.1°. Conclusions: This device fulfills the stringent requirements for operations in cryogenic space experiments, such as the forthcoming PILOT, BOOMERanG and LSPE.

Crystallization of Chicken Egg-White Lysozyme from Ammonium Sulfate

NASA Technical Reports Server (NTRS)

Forsythe, Elizabeth L.; Snell, Edward H.; Pusey, Marc L.

1997-01-01

Chicken egg-white lysozyme was crystallized from ammonium sulfate over the pH range 4.0-7.8, with protein concentrations from 100 to 150 mg/ml. Crystals were obtained by vapor-diffusion or batch-crystallization methods. The protein crystallized in two morphologies with an apparent morphology dependence on temperature and protein concentration. In general, tetragonal crystals could be grown by lowering the protein concentration or temperature. Increasing the temperature or protein concentration resulted in the growth of orthorhombic crystals. Representative crystals of each morphology were selected for X-ray analysis. The tetragonal crystals belonged to the P4(sub 3)2(sub 1)2 space group with crystals grown at ph 4.4 having unit-cell dimensions of a = b = 78.7 1, c=38.6 A and diffracting to beyond 2.0 A. The orthorhombic crystals, grown at pH 4.8, were of space group P2(sub 1)2(sub 1)2 and had unit-cell dimensions of a = 30.51, b = 56.51 and c = 73.62 A.

Radiation resistance of nonlinear crystals at a wavelength of 9.55 {mu}m

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

Andreev, Yu M; Voevodin, V G; Badikov, Valerii V

2001-12-31

The results of radiation resistance measurements for twelve nonlinear crystals are presented. The crystals include the well-known nonlinear CdGeAs{sub 2}, ZnGeP{sub 2}, AgGaSe{sub 2}, GaSe, AgGaS{sub 2}, and Ag{sub 3}AsS{sub 3} crystals operating in the middle IR range, new mixed AgGaGeS{sub 4} and Cd{sub 0.35}Hg{sub 0.65}Ga{sub 2}S{sub 4} crystals, two-phase (orange and yellow) HgGa{sub 2}S{sub 4} crystal, and the doped GaSe:In crystal. The mixed crystals and the two-phase HgGa{sub 2}S{sub 4} crystal are transparent in the range from 0.4 - 0.5 to 11.5 - 14.5 {mu}m. The measurements were performed using a pulsed single-mode highly stability TEA CO{sub 2} lasermore » with an output pulse duration of {approx}30 ns. The damage thresholds of new nonlinear AgGaGeS{sub 4} and Cd {sub 0.35}Hg{sub 0.65}Ga{sub 2}S{sub 4} crystals and of the HgGa{sub 2}S{sub 4} crystal (the orange and yellow phases) were found to be 1.5 - 2.2 times higher than for the crystals operating in the middle IR range. (interaction of laser radiation with matter. laser plasma)« less

Luminescence from edge fracture in shocked lithium fluoride crystals

DOE PAGES

Turley, W. D.; Stevens, G. D.; Capelle, G. A.; ...

2013-04-03

Light emitted from a [100] lithium fluoride crystal was characterized under shock wave compression to 28 GPa followed by complete stress release at the edges. We examined the light using time-gated optical spectrometry and imaging, time-resolved optical emission measurements, and hydrodynamic modeling. The shock arrival at the circumference of the crystal was delayed relative to the center so that the two regions could be studied at different times. The majority of the light emission originated when the shock waves released at the circumference of the crystal. Unlike previously reported results for shocked lithium fluoride, we found that the light spectrummore » is not strictly broad band, but has spectral lines associated with atomic lithium in addition to a broad band background. Also, the emission spectrum depends strongly on the gas surrounding the sample. Based on our observations, the line emission appears to be related to fracture of the lithium fluoride crystal from the shock wave releasing at the edges. Moreover, experimenters frequently utilize lithium fluoride crystals as transparent windows for observing shock compressed samples. Because of the experimental geometries used, the shock wave in such cases often reaches the circumference of the window at nearly the same moment as when it reaches the center of the sample-window interface. Light generated at the circumference could contaminate the measurement at the interface when this light scatters into the observed region. Finally, this background light may be reduced or avoided using experimental geometries which delay the arrival of the shock wave at the edges of the crystal.« less

Synthesis, structural, optical and thermal studies of an organic nonlinear optical 4-aminopyridinium maleate single crystal.

PubMed

Pandi, P; Peramaiyan, G; Kumar, M Krishna; Kumar, R Mohan; Jayavel, R

2012-03-01

Synthesis and growth of a novel organic nonlinear optical (NLO) crystal of 4-aminopyridinium maleate (4APM) in larger size by the slow evaporation solution growth technique are reported. Single crystal and powder X-ray diffraction analyses reveal that 4APM crystallizes in monoclinic system with space group P2(1) with cell parameters a=8.140(4)Å, b=5.457(5)Å, c=10.926(10)Å and volume=481.4(7)Å(3). The grown crystal has been characterized by Fourier transform infrared and UV-visible spectral analyses. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) have been carried out to study its thermal properties. Dielectric measurements have been carried out to study the distribution of charges within the crystal. The mechanical strength of the crystal has been studied by using Vickers' microhardness test. The etching studies have been carried out on the grown crystal. The Kurtz and Perry powder SHG technique confirms the NLO property of the grown crystal and the SHG efficiency of 4APM was found to be 4.8 times greater than that of KDP crystal. Copyright © 2011 Elsevier B.V. All rights reserved.

Crystal growth and optical characteristics of beryllium-free polyphosphate, KLa(PO3)4, a possible deep-ultraviolet nonlinear optical crystal

NASA Astrophysics Data System (ADS)

Shan, Pai; Sun, Tongqing; Chen, Hong; Liu, Hongde; Chen, Shaolin; Liu, Xuanwen; Kong, Yongfa; Xu, Jingjun

2016-04-01

Deep-ultraviolet nonlinear optical crystals are of great importance as key materials in generating coherent light with wavelength below 200 nm through cascaded frequency conversion of solid-state lasers. However, the solely usable crystal in practice, KBe2BO3F2 (KBBF), is still commercially unavailable because of the high toxicity of beryllium-containing and the extreme difficulty of crystal growth. Here, we report the crystal growth and characteristics of an beryllium-free polyphosphate, KLa(PO3)4. Centimeter-sized single crystals have been easily obtained by the flux method and slow-cooling technique. The second-harmonic generation efficiency of KLa(PO3)4 powder is 0.7 times that of KH2PO4; moreover, the KLa(PO3)4 crystal is phase-matchable. Remarkably, the KLa(PO3)4 crystal exhibits an absorption edge of 162 nm, which is the shortest among phase-matchable phosphates so far. These attributes make KLa(PO3)4 a possible deep-ultraviolet nonlinear optical crystal. An analysis of the dipole moments of the polyhedra and theoretical calculations by density functional theory were made to elucidate the structure-properties relationships of KLa(PO3)4.

Photovoltaic spatial solitons affected by a resistor in the external circuit

NASA Astrophysics Data System (ADS)

Wang, Xiao Sheng; She, Wei Long

2002-09-01

We have found that the FWHM of one-dimensional photovoltaic spatial soliton is modified by the space-charge field in the crystal, which can be controlled by a resistor in the external circuit. In this case, the photovoltaic contribution of a background beam is taken into account. In a crystal with a positive perturbation of refractive index, the FWHM of dark soliton decreases with the resistance of the resistor, while the FWHM of bright soliton increases with the resistance. Furthermore, when R (the ratio of the effective Glass constant of a signal beam over a background beam) is higher than 1, we can switch a dark soliton to a bright soliton by decreasing the resistance or vice versa. During such process, both the wavelengths and the intensities of the signal beam and the background beam are kept unchanged.

Easy approach to assembling a biomimetic color film with tunable structural colors.

PubMed

Wang, Wentao; Tang, Bingtao; Ma, Wei; Zhang, Jian; Ju, Benzhi; Zhang, Shufen

2015-06-01

The self-assembly of silica microspheres into a close-packed array is a simple method of fabricating three-dimensional photonic crystal structural color films. However, the color is very dull because of the interferences of scattering and background light. In this study, we added a small quantity of surface-modified carbon black (CB) to the system of colloidal silica in n-propanol. The use of n-propanol as a dispersant is beneficial to the rapid development of photonic crystal films during the process of dip-coating. The doping of CB into silica microspheres can absorb background and scattering light, resulting in vivid structural colors.

Applications of thin-film sandwich crystallization platforms

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

Axford, Danny, E-mail: danny.axford@diamond.ac.uk; Aller, Pierre; Sanchez-Weatherby, Juan

2016-03-24

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

[Growth of codoped CdWO4 crystals by Bridgman method and their optical spectra].

PubMed

Yu, Can; Xia, Hai-Ping; Wang, Dong-Jie; Chen, Hong-Bing

2011-09-01

The CdWO4 crystals with good quality in the size of Phi25 mm x 120 mm, doped with Co in 0.5% molar fraction in the raw composition, were grown by the Bridgman method by taking -70 degrees C x cm(-1) of solid-liquid interface and -0.50 mm x h(-1) growth rate. The crystal presents transparence and deep blue. The X-ray diffraction (XRD) was used to characterize the crystals. Three absorption peaks at 518, 564 and 655 nm respectively, which are attributed to the overlapping of 4 T1 (4F) --> 4A2 (4F) and 4 T1 (4F) --> 4 T1 (4P) of Co2+ octahedrons, and a wide band centered at 1 863 nm, which is attributed to 4Ti (4F) --> 4 T2 (4F), was observed. The absorption results indicated that the Co ions presented +2 valence in crystal and located within the distorted oxygen octahedrons. The crystal-field parameter D(q) and the Racah parameter B were estimated to be 990 and 726.3 cm(-1) respectively based on the absorption spectra. A fluorescence emission at 778 nm (4T1 (4P) --> 4 T1 (4F)) for codoped CdWO4 crystals was observed under excitation by 520 nm light. It can be deduced from the changes in absorption and emission intensity of different parts of crystal that the concentration of Co2+ ion in crystal increased along growing direction and the effective distribution coefficient of Co2+ ion in CdWO4 crystal is less than 1.

Effect of solvents on the bulk growth of 4-aminobenzophenone single crystals: A potential material for blue and green lasers

NASA Astrophysics Data System (ADS)

Natarajan, V.; Usharani, S.; Arivanandhan, M.; Anandan, P.; Hayakawa, Y.

2015-06-01

Although 4-aminobenzophenone (4-ABP) is the best derivative of benzophenone with 260 times higher second harmonic generation (SHG) efficiency than potassium dihydrogen phosphate (KDP), growth of high quality bulk crystal still remains a difficult task. In the present work, the effect of solvents on solubility and growth aspects of 4-ABP was investigated to grow inclusion free 4-ABP crystals. The growth processes were discussed based on solute-solvent interaction in two different growth media of ethyl acetate and ethanol. The growth rate and thereby solvent inclusions are relatively higher in ethyl acetate grown crystal than the crystal grown from ethanol. The structural, thermal and optical properties of 4-ABP crystals were studied. The enthalpy of 4-ABP melting process was estimated from differential thermal analysis. The optical transmission study shows that 4-ABP crystals grown from ethanol has high transparency compared to ethyl acetate grown sample due to solvent inclusion in the later crystal.

Synthesis and Structural Features of [4,4'-Diisopropoxyester-2,2'-bipyridine], [Dichloro(4,4'-diisopropoxyester-2,2'-bi-pyridine)-platinum(ii)] and Its Dichloromethane Solvated Pseudo-Polymorph: Versatile Supramolecular Interactions

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

Browning, Charles; Nesterov, Vladimir N.; Wang, Xiaoping

We report that the organic ligand 4,4'-diisopropoxyester-2,2'-bipyridine, C 18H 20N 2O 4 (1), crystallizes in the triclinic crystal system P-1 and the molecule occupies a special position in the unit cell. In the crystal, molecules form stacks with partial overlapping of the pyridine rings. The Pt(II) dichloro complex of 1 crystallizes from a mixture of ethanol/hexane and from dichloromethane to form orange and yellow crystals, respectively. The orange non-solvated crystals of the (bipyridine)(dichloro)platinum(II) complex C 18H 20N 2O 4PtCl 2 (2) crystallize in the triclinic crystal system P-1 as well with two independent molecules in the unit cell. In themore » crystal packing, molecules form two types of dimers with Pt1 ··· Pt1A and Pt2···Pt2A distances of 3.478 and 5.186 angstrom respectively. The yellow crystals, as a solvated pseudo-polymorph C 18H 20N 2O 4PtCl 2·1.5 CH 2Cl 2 (3) also crystallize in the triclinic crystal system P-1 with two independent molecules in the unit cell. In the crystal packing, molecules form Pt2 ···Pt1 ···Pt1A ···Pt2A intermolecular contacts with alternating distances 3.501 and 3.431 angstrom, respectively, forming infinite chains. Graphical Abstract The dichloro(bipyridine)platinum complex, dichloro(4,4'-diisopropoxyester-2,2'-bipyridine)platinum(II), forms single crystals as a stable non-solvated form and a solvated polymorph with dramatically different supramolecular structure and short contacts.« less

Synthesis and Structural Features of [4,4'-Diisopropoxyester-2,2'-bipyridine], [Dichloro(4,4'-diisopropoxyester-2,2'-bi-pyridine)-platinum(ii)] and Its Dichloromethane Solvated Pseudo-Polymorph: Versatile Supramolecular Interactions

DOE PAGES

Browning, Charles; Nesterov, Vladimir N.; Wang, Xiaoping; ...

2015-06-03

We report that the organic ligand 4,4'-diisopropoxyester-2,2'-bipyridine, C 18H 20N 2O 4 (1), crystallizes in the triclinic crystal system P-1 and the molecule occupies a special position in the unit cell. In the crystal, molecules form stacks with partial overlapping of the pyridine rings. The Pt(II) dichloro complex of 1 crystallizes from a mixture of ethanol/hexane and from dichloromethane to form orange and yellow crystals, respectively. The orange non-solvated crystals of the (bipyridine)(dichloro)platinum(II) complex C 18H 20N 2O 4PtCl 2 (2) crystallize in the triclinic crystal system P-1 as well with two independent molecules in the unit cell. In themore » crystal packing, molecules form two types of dimers with Pt1 ··· Pt1A and Pt2···Pt2A distances of 3.478 and 5.186 angstrom respectively. The yellow crystals, as a solvated pseudo-polymorph C 18H 20N 2O 4PtCl 2·1.5 CH 2Cl 2 (3) also crystallize in the triclinic crystal system P-1 with two independent molecules in the unit cell. In the crystal packing, molecules form Pt2 ···Pt1 ···Pt1A ···Pt2A intermolecular contacts with alternating distances 3.501 and 3.431 angstrom, respectively, forming infinite chains. Graphical Abstract The dichloro(bipyridine)platinum complex, dichloro(4,4'-diisopropoxyester-2,2'-bipyridine)platinum(II), forms single crystals as a stable non-solvated form and a solvated polymorph with dramatically different supramolecular structure and short contacts.« less

Improved Success of Sparse Matrix Protein Crystallization Screening with Heterogeneous Nucleating Agents

PubMed Central

Thakur, Anil S.; Robin, Gautier; Guncar, Gregor; Saunders, Neil F. W.; Newman, Janet; Martin, Jennifer L.; Kobe, Bostjan

2007-01-01

Background Crystallization is a major bottleneck in the process of macromolecular structure determination by X-ray crystallography. Successful crystallization requires the formation of nuclei and their subsequent growth to crystals of suitable size. Crystal growth generally occurs spontaneously in a supersaturated solution as a result of homogenous nucleation. However, in a typical sparse matrix screening experiment, precipitant and protein concentration are not sampled extensively, and supersaturation conditions suitable for nucleation are often missed. Methodology/Principal Findings We tested the effect of nine potential heterogenous nucleating agents on crystallization of ten test proteins in a sparse matrix screen. Several nucleating agents induced crystal formation under conditions where no crystallization occurred in the absence of the nucleating agent. Four nucleating agents: dried seaweed; horse hair; cellulose and hydroxyapatite, had a considerable overall positive effect on crystallization success. This effect was further enhanced when these nucleating agents were used in combination with each other. Conclusions/Significance Our results suggest that the addition of heterogeneous nucleating agents increases the chances of crystal formation when using sparse matrix screens. PMID:17971854

In situ data collection and structure refinement from microcapillary protein crystallization

PubMed Central

Yadav, Maneesh K.; Gerdts, Cory J.; Sanishvili, Ruslan; Smith, Ward W.; Roach, L. Spencer; Ismagilov, Rustem F.; Kuhn, Peter; Stevens, Raymond C.

2007-01-01

In situ X-ray data collection has the potential to eliminate the challenging task of mounting and cryocooling often fragile protein crystals, reducing a major bottleneck in the structure determination process. An apparatus used to grow protein crystals in capillaries and to compare the background X-ray scattering of the components, including thin-walled glass capillaries against Teflon, and various fluorocarbon oils against each other, is described. Using thaumatin as a test case at 1.8 Å resolution, this study demonstrates that high-resolution electron density maps and refined models can be obtained from in situ diffraction of crystals grown in microcapillaries. PMID:17468785

Intercalating dyes for enhanced contrast in second-harmonic generation imaging of protein crystals

PubMed Central

Newman, Justin A.; Scarborough, Nicole M.; Pogranichniy, Nicholas R.; Shrestha, Rashmi K.; Closser, Richard G.; Das, Chittaranjan; Simpson, Garth J.

2015-01-01

The second-harmonic generation (SHG) activity of protein crystals was found to be enhanced by up to ∼1000-fold by the intercalation of SHG phores within the crystal lattice. Unlike the intercalation of fluorophores, the SHG phores produced no significant background SHG from solvated dye or from dye intercalated into amorphous aggregates. The polarization-dependent SHG is consistent with the chromophores adopting the symmetry of the crystal lattice. In addition, the degree of enhancement for different symmetries of dyes is consistent with theoretical predictions based on the molecular nonlinear optical response. Kinetics studies indicate that intercalation arises over a timeframe of several minutes in lysozyme, with detectable enhancements within seconds. These results provide a potential means to increase the overall diversity of protein crystals and crystal sizes amenable to characterization by SHG microscopy. PMID:26143918

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

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.

Crystal growth and optical characteristics of beryllium-free polyphosphate, KLa(PO3)4, a possible deep-ultraviolet nonlinear optical crystal

PubMed Central

Shan, Pai; Sun, Tongqing; Chen, Hong; Liu, Hongde; Chen, Shaolin; Liu, Xuanwen; Kong, Yongfa; Xu, Jingjun

2016-01-01

Deep-ultraviolet nonlinear optical crystals are of great importance as key materials in generating coherent light with wavelength below 200 nm through cascaded frequency conversion of solid-state lasers. However, the solely usable crystal in practice, KBe2BO3F2 (KBBF), is still commercially unavailable because of the high toxicity of beryllium-containing and the extreme difficulty of crystal growth. Here, we report the crystal growth and characteristics of an beryllium-free polyphosphate, KLa(PO3)4. Centimeter-sized single crystals have been easily obtained by the flux method and slow-cooling technique. The second-harmonic generation efficiency of KLa(PO3)4 powder is 0.7 times that of KH2PO4; moreover, the KLa(PO3)4 crystal is phase-matchable. Remarkably, the KLa(PO3)4 crystal exhibits an absorption edge of 162 nm, which is the shortest among phase-matchable phosphates so far. These attributes make KLa(PO3)4 a possible deep-ultraviolet nonlinear optical crystal. An analysis of the dipole moments of the polyhedra and theoretical calculations by density functional theory were made to elucidate the structure-properties relationships of KLa(PO3)4. PMID:27126353

Design and Performance of a 1 mm3 Resolution Clinical PET System Comprising 3-D Position Sensitive Scintillation Detectors.

PubMed

Hsu, David F C; Freese, David L; Reynolds, Paul D; Innes, Derek R; Levin, Craig S

2018-04-01

We are developing a 1-mm 3 resolution, high-sensitivity positron emission tomography (PET) system for loco-regional cancer imaging. The completed system will comprise two cm detector panels and contain 4 608 position sensitive avalanche photodiodes (PSAPDs) coupled to arrays of mm 3 LYSO crystal elements for a total of 294 912 crystal elements. For the first time, this paper summarizes the design and reports the performance of a significant portion of the final clinical PET system, comprising 1 536 PSAPDs, 98 304 crystal elements, and an active field-of-view (FOV) of cm. The sub-system performance parameters, such as energy, time, and spatial resolutions are predictive of the performance of the final system due to the modular design. Analysis of the multiplexed crystal flood histograms shows 84% of the crystal elements have>99% crystal identification accuracy. The 511 keV photopeak energy resolution was 11.34±0.06% full-width half maximum (FWHM), and coincidence timing resolution was 13.92 ± 0.01 ns FWHM at 511 keV. The spatial resolution was measured using maximum likelihood expectation maximization reconstruction of a grid of point sources suspended in warm background. The averaged resolution over the central 6 cm of the FOV is 1.01 ± 0.13 mm in the X-direction, 1.84 ± 0.20 mm in the Y-direction, and 0.84 ± 0.11 mm in the Z-direction. Quantitative analysis of acquired micro-Derenzo phantom images shows better than 1.2 mm resolution at the center of the FOV, with subsequent resolution degradation in the y-direction toward the edge of the FOV caused by limited angle tomography effects.

On the synthesis of AlPO4-21 molecular sieve by vapor phase transport method and its phase transformation to AlPO4-15 molecular sieve

NASA Astrophysics Data System (ADS)

Shao, Hui; Chen, Jingjing; Chen, Xia; Leng, Yixin; Zhong, Jing

2015-04-01

An experimental design was applied to the synthesis of AlPO4-21 molecular sieve (AWO structure) by vapor phase transport (VPT) method, using tetramethylguanidine (TMG) as the template. In this study, the effects of crystallization time, crystallization temperature, phosphor content, template content and water content in the synthesis gel were investigated. The materials obtained were characterized by X-ray diffraction, scanning electron microscopy and fourier transform infrared spectroscopy (FT-IR). Microstructural analysis of the crystal growth in vapor synthetic conditions revealed a revised crystal growth route from zeolite AlPO4-21 to AlPO4-15 in the presence of the TMG. Homogenous hexagonal prism AlPO4-21 crystals with size of 7 × 3 μm were synthesized at a lower temperature (120 °C), which were completely different from the typical tabular parallelogram crystallization microstructure of AlPO4-21 phase. The crystals were transformed into AlPO4-21 phase with higher crystallization temperature, longer crystallization time, higher P2O5/Al2O3 ratio and higher TMG/Al2O3 ratio.

Resonant Soft X-ray Scattering studies with Transition Edge Sensors

NASA Astrophysics Data System (ADS)

Fang, Yizhi; Lee, Sangjun; de La Pena, Gilberto; Sun, Xiaolan; Rodolakis, Fanny; McChesney, Jessica; Fowler, Joe; Joe, Young Il; Doriese, William; Morgan, Kelsey; Swetz, Daniel; Ullom, Joel; Abbamonte, Peter

Resonant Soft X-ray has been one of the key techniques to study charge orders in high Tc cuperates. To solve the issue of unwanted enhancement of inelastic florescence background at resonance, we have developed an energy-resolving superconducting Transition-Edge Sensor microcalorimeters. These superconducting sensors obtain exquisite energy resolution by exploiting the superconducting-to-normal transition to photon energy and by operating at cryogenic temperatures ( 70 mK) where thermal noise is minimal. This TES has demonstrated 1.0 eV resolution below 1 keV. We present first results using this detector to study the (002) Bragg peak and specular elastic scattering from a single crystal of stripe-ordered La 2 - x Bax CuO4 (x=0.125). Use of this detector for studying excitations and rejecting background fluorescence will be discussed.

Crystal growth, spectral, structural and optical studies of π-conjugated stilbazolium crystal: 4-bromobenzaldehyde-4'-N'-methylstilbazolium tosylate.

PubMed

Krishna Kumar, M; Sudhahar, S; Bhagavannarayana, G; Mohan Kumar, R

2014-05-05

Nonlinear optical (NLO) organic compound, 4-bromobenzaldehyde-4'-N'-methylstilbazolium tosylate was synthesized by reflux method. The formation of molecular complex was confirmed from (1)H NMR, FT-IR and FT-Raman spectral analyses. The single crystals were grown by slow evaporation solution growth method and the crystal structure and atomic packing of grown crystal was identified. The morphology and growth axis of grown crystal were determined. The crystal perfection was analyzed using high resolution X-ray diffraction study on (001) plane. Thermal stability, decomposition stages and melting point of the grown crystal were analyzed. The optical absorption coefficient (α) and energy band gap (E(g)) of the crystal were determined using UV-visible absorption studies. Second harmonic generation efficiency of the grown crystal was examined by Kurtz powder method with different particle size using 1064 nm laser. Laser induced damage threshold study was carried out for the grown crystal using Nd:YAG laser. Copyright © 2014 Elsevier B.V. All rights reserved.

Investigation of Optical and Electrical Properties of Wide Band Gap Materials

DTIC Science & Technology

1976-06-01

porous and heterogeneous. 22 IF 3. CRYSTAL GROWTH OF HgS A. Background fI’ Mercury sulfide is a wide bandgap semiconductor which is of considerable...I24 I 23 Mercury sulfide exists in two modifications, cinnabar (a-HgS) and metacinnabar (0-HgS). The a phase crystallizes in an unusual, dihedrally...5.817 ) at 26 °C, with Eg = -0.15 eV. An early technique, reported by Hamilton 31, on the synthesis of single crystals of the sulphides of Zn, Cd

Efficient Incorporation of Mg in Solution Grown GaN Crystals

NASA Astrophysics Data System (ADS)

Freitas, Jaime A., Jr.; Feigelson, Boris N.; Anderson, Travis J.

2013-11-01

Detailed spectrometry and optical spectroscopy studies carried out on GaN crystals grown in solution detect and identify Mg as the dominant shallow acceptor. Selective etching of crystals with higher Mg levels than that of the donor concentration background indicates that Mg acceptors incorporate preferentially in the N-polar face. Electrical transport measurements verified an efficient incorporation and activation of the Mg acceptors. These results suggest that this growth method has the potential to produce p-type doped epitaxial layers or p-type substrates characterized by high hole concentration and low defect density.

Single crystal growth and characterization of pure and sodium-modified copper tartrate

NASA Astrophysics Data System (ADS)

Quasim, I.; Firdous, A.; Want, B.; Khosa, S. K.; Kotru, P. N.

2008-12-01

Single crystal growth of pure and modified copper tartrate crystals bearing composition (Cu) x(Na) yC 4H 4O 6· nH 2O (where x=1, 0.77, 0.65; y=0, 0.23, 0.35) is achieved using gel technique. The optimum conditions required for the growth of these crystals are worked out. The morphological development of these crystals is studied using optical and scanning electron microscopy. The dominant habit faces of the grown copper tartrate crystals are (0 0 1) and (1 1 1). Calculation of the cell parameters using CRYSFIRE software suggests that the pure copper tartrate crystal belongs to orthorhombic system with space group P2 1/c whereas the modified copper tartrate falls under tetragonal system with the space group P4 2/nbc. The external morphological development is shown to remain unaffected in the modified copper tartrate. The stoichiometric composition of the crystals is established by EDAX analysis, CH analysis, FTIR spectroscopy and thermoanalytical techniques. Thermal analysis of the grown crystals suggests that pure copper tartrate is thermally stable up to 42.84 °C whereas the modified copper tartrate crystals are stable only up to 33.11 and 25.11 °C. Calculation of the percentage weight loss from the thermogram supplemented by EDAX/CH analysis and FTIR spectroscopy suggest that the chemical formula of pure copper tartrate crystal is CuC 4H 4O 6·3H 2O whereas the chemical formula for the modified copper tartrate crystals is (Cu) 0.77(Na) 0.23C 4H 4O 6·3H 2O and (Cu) 0.65(Na) 0.35 C 4H 4O 6·H 2O.

Vivid structural colors with low angle dependence from long-range ordered photonic crystal films.

PubMed

Su, Xin; Xia, Hongbo; Zhang, Shufen; Tang, Bingtao; Wu, Suli

2017-03-02

Structural colored materials have attracted increasing attention due to their vivid color effects and non-photobleaching characteristics. However, the angle dependence of these structural colors severely restricts their practical applications, for example, in display and sensing devices. Here, a new strategy for obtaining low angle dependent structural colors is demonstrated by fabricating long-range ordered photonic crystal films. By using spheres with high refractive indices as building blocks, the angle dependence of the obtained colors has been strongly suppressed. Green, golden yellow and red structural colored films with low angle dependence were obtained by using 145 nm, 165 nm and 187 nm Cu 2 O spheres as building blocks, respectively. SEM images confirmed the long-range highly ordered arrays of the Cu 2 O photonic crystal films. Reflectance spectra and digital photographs clearly demonstrate the low angle dependence of these structural colors, which is in sharp comparison with the case of polystyrene (PS) and SiO 2 photonic crystal films. Furthermore, these structural colors are vivid with high color saturation, not only under black background, but also under white background and natural light without adding any light-absorbing agents. These low angle dependent structural colors endow Cu 2 O photonic crystal films with great potential in practical applications. Our findings may broaden the strategies for the design and fabrication of angle independent structural colored materials.

Process development and characterization of centrosymmetric semiorganic nonlinear optical crystal: 4-dimethylaminopyridine potassium chloride

NASA Astrophysics Data System (ADS)

Johnson, J.; Srineevasan, R.; Sivavishnu, D.

2018-06-01

Centrosymmetric semiorganic crystal 4-dimethylaminopyridine potassium chloride (4-DMAPKC) has been grown successfully by using slow evaporation solution growth technique. Powder x-ray diffraction shows the 4-DMAPKC crystal has good crystalline nature. Single crystal XRD shows that the grown 4-DMAPKC is cubic crystal system with cell parameters a = 3.09 Å, b = 3.09 Å, c = 3.09 Å. Investigation has been carried out to assign the Vibrational frequencies of the grown crystal by FTIR spectral studies. UVsbnd Visible NIR optical absorption spectral studies in the range of 200-1100 nm shows low absorption in UVsbnd Visible region with lower cutoff wave length at 261 nm and optical band gap energy was found as Eg = 5.52 eV. Optically transmittance spectral shows 4-DMAPKC crystal is very good transparency in UV-Visible NIR region. Thermogravimetry and differential thermal (TG-DTA) analysis were carried out. Dielectric studies of as grown crystal sample exhibit low dielectric constant and loss at higher frequencies and attests the nonlinear optical activity. Micro hardness studies of as grown crystal were discussed. Second harmonic generation (SHG) efficiency of the 4-DMAPKC is 0.69 times as that of KDP.

Dissolving and melting phenomena of inorganic and organic crystals by addition of third or second components

NASA Astrophysics Data System (ADS)

Funakoshi, Kunio; Negishi, Rina; Nakagawa, Hiroshi; Kawasaki, Rentaro

2017-06-01

Dissolution of potassium sulphate (K2SO4) crystals was decelerated or stopped since the trivalent chrome ions (Cr(III)) or the iron ions were added into a K2SO4 aqueous solution, but inhibition mechanism of crystal dissolving by additives is not discussed well. Moreover, the melting inhibition of organic compound crystals by addition of the second components is not reported. In this study, inorganic or organic compound crystals are dissolved in a solution added the third component or were melted in a melt added the second one, and the dissolving and melting inhibition phenomena of the inorganic and organic crystals with additives are discussed. The dissolving rates of K2SO4 crystals decreased with the increasing of the amount of Cr(III) added into an K2SO4 unsaturated solution. The melting rates of m-chloronitrobenzene (CNB) crystals were also decreased by addition of p-CNB. The dissolving rates of a K2SO4 mother crystal and the melting rates of a m-CNB mother crystal were scattered during experiments and the dissolving and the melting phenomena would be caused by adsorption and detachments of additives on and from crystal surfaces.

Tips pentacene crystal alignment for improving performance of solution processed organic thin film transistors

NASA Astrophysics Data System (ADS)

He, Zhengran

A newly-developed p-type organic semiconductor 6,13-bis (triisopropylsilylethynyl) pentacene (TIPS pentacene) demonstrates various advantages such as high mobility, air stability and solution processibility, but at the same time its application is restricted by major issues, such as crystal misorientation and performance variation of organic thin-film transistors (OTFTs). This dissertation demonstrates several different approaches to address these issues. As a result, both crystal orientation and areal coverage can be effectively improved, leading to an enhancement of average mobility and performance consistency of OTFTs. Chapter 1 presents an introduction and background of this dissertation. Chapter 2 explores the usage of inorganic silica nanoparticles to manipulate the morphology of TIPS pentacene thin films and the performance of solution-processed organic OTFTs. The resultant drop-cast films yield improved morphological uniformity at ~10% SiO2 loading, which also leads to a 3-fold increase in average mobility and nearly 4-times reduction in the ratio of standard deviation of mobility (μStdev) to average mobility (μAvg). The experimental results suggest that the SiO2 nanoparticles mostly aggregate at TIPS pentacene grain boundaries, and that 10% nanoparticle concentration effectively reduces the undesirable crystal misorientation without considerably compromising TIPS pentacene crystallinity. Chapter 3 discusses the utilization of air flow to effectively reduce the TIPS pentacene crystal anisotropy and enhance performance consistency in OTFTs. Under air-flow navigation (AFN), TIPS pentacene forms thin films with improved crystal orientation and increased areal coverage, which subsequently lead to a four-fold increase of average hole mobility and one order of magnitude enhancement in performance consistency. Chapter 4 investigates the critical roles of lateral and vertical phase separation in the performance of the next-generation organic and hybrid electronic devices. A novel method is demonstrated here to switch between lateral and vertical phase separation in semiconducting TIPS pentacene/ polymer blend films by simply varying the alkyl length of the polyacrylate polymer component. The phase separation modes depend on intermolecular interactions between small molecule TIPS pentacene and polymer additives. The blend film with a dominant vertical phase separation exhibits a significant enhancement in average mobility and performance consistency of organic OTFTs. Chapter 5 demonstrates an effective approach to improve both charge transport and performance consistency in solution-processed OTFTs by blending TIPS pentacene with a series of small-molecule additives: 4-butylbenzoic acid (BBA), 4-hexylbenzoic acid (HBA), and 4-octylbenzoic acid (OBA). These three small molecules share a benzoic acid moiety, but have different length of hydrophobic tails. The self-assembled interfacial layer of small molecules on the gate oxide surface leads to uniform deposition of TIPS pentacene crystal seeds and facilitates TIPS pentacene to grow along the tilted orientation of substrate, which results in a film of enhanced crystal orientation and areal coverage. OTFTs based on TIPS pentacene/small molecule blends demonstrate greatly improved average hole mobility and performance consistency, which correlates with the length of hydrophobic tail of the small-molecule additives. Chapter 6 summarizes the conclusions of this dissertation and the related future work.

Managing SRS competition in a miniature visible Nd:YVO4/BaWO4 Raman laser.

PubMed

Li, Xiaoli; Lee, Andrew J; Huo, Yujing; Zhang, Huaijin; Wang, Jiyang; Piper, James A; Pask, Helen M; Spence, David J

2012-08-13

We demonstrate the operation of a compact and efficient continuous wave (CW) self-Raman laser utilizing a Nd:YVO4 gain crystal and BaWO4 Raman crystal, generating yellow emission at 590 nm. We investigate the competition that occurs between Stokes lines in the Nd:YVO4 and BaWO4 crystals, and within the BaWO4 crystal itself. Through careful consideration of crystal length and orientation, we are able to suppress competition between Stokes lines, and generate pure yellow emission at 590 nm with output power of 194 mW for just 3.8 W pump power.

Applications of thin-film sandwich crystallization platforms.

PubMed

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

2016-04-01

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

A top-down approach to crystal engineering of a racemic Δ2-isoxazoline.

PubMed

Lombardo, Giuseppe M; Rescifina, Antonio; Chiacchio, Ugo; Bacchi, Alessia; Punzo, Francesco

2014-02-01

The crystal structure of racemic dimethyl (4RS,5RS)-3-(4-nitrophenyl)-4,5-dihydroisoxazole-4,5-dicarboxylate, C13H12N2O7, has been determined by single-crystal X-ray diffraction. By analysing the degree of growth of the morphologically important crystal faces, a ranking of the most relevant non-covalent interactions determining the crystal structure can be inferred. The morphological information is considered with an approach opposite to the conventional one: instead of searching inside the structure for the potential key interactions and using them to calculate the crystal habit, the observed crystal morphology is used to define the preferential lines of growth of the crystal, and then this information is interpreted by means of density functional theory (DFT) calculations. Comparison with the X-ray structure confirms the validity of the strategy, thus suggesting this top-down approach to be a useful tool for crystal engineering.

Morphology and the Strength of Intermolecular Contact in Protein Crystals

NASA Technical Reports Server (NTRS)

Matsuura, Yoshiki; Chernov, Alexander A.

2002-01-01

The strengths of intermolecular contacts (macrobonds) in four lysozyme crystals were estimated based on the strengths of individual intermolecular interatomic interaction pairs. The periodic bond chain of these macrobonds accounts for the morphology of protein crystals as shown previously. Further in this paper, the surface area of contact, polar coordinate representation of contact site, Coulombic contribution on the macrobond strength, and the surface energy of the crystal have been evaluated. Comparing location of intermolecular contacts in different polymorphic crystal modifications, we show that these contacts can form a wide variety of patches on the molecular surface. The patches are located practically everywhere on this surface except for the concave active site. The contacts frequently include water molecules, with specific intermolecular hydrogen-bonds on the background of non-specific attractive interactions. The strengths of macrobonds are also compared to those of other protein complex systems. Making use of the contact strengths and taking into account bond hydration we also estimated crystal-water interfacial energies for different crystal faces.

Inkjet Printing Based Mono-layered Photonic Crystal Patterning for Anti-counterfeiting Structural Colors.

PubMed

Nam, Hyunmoon; Song, Kyungjun; Ha, Dogyeong; Kim, Taesung

2016-08-04

Photonic crystal structures can be created to manipulate electromagnetic waves so that many studies have focused on designing photonic band-gaps for various applications including sensors, LEDs, lasers, and optical fibers. Here, we show that mono-layered, self-assembled photonic crystals (SAPCs) fabricated by using an inkjet printer exhibit extremely weak structural colors and multiple colorful holograms so that they can be utilized in anti-counterfeit measures. We demonstrate that SAPC patterns on a white background are covert under daylight, such that pattern detection can be avoided, but they become overt in a simple manner under strong illumination with smartphone flash light and/or on a black background, showing remarkable potential for anti-counterfeit techniques. Besides, we demonstrate that SAPCs yield different RGB histograms that depend on viewing angles and pattern densities, thus enhancing their cryptographic capabilities. Hence, the structural colorations designed by inkjet printers would not only produce optical holograms for the simple authentication of many items and products but also enable a high-secure anti-counterfeit technique.

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.

Inkjet Printing Based Mono-layered Photonic Crystal Patterning for Anti-counterfeiting Structural Colors

NASA Astrophysics Data System (ADS)

Nam, Hyunmoon; Song, Kyungjun; Ha, Dogyeong; Kim, Taesung

2016-08-01

Photonic crystal structures can be created to manipulate electromagnetic waves so that many studies have focused on designing photonic band-gaps for various applications including sensors, LEDs, lasers, and optical fibers. Here, we show that mono-layered, self-assembled photonic crystals (SAPCs) fabricated by using an inkjet printer exhibit extremely weak structural colors and multiple colorful holograms so that they can be utilized in anti-counterfeit measures. We demonstrate that SAPC patterns on a white background are covert under daylight, such that pattern detection can be avoided, but they become overt in a simple manner under strong illumination with smartphone flash light and/or on a black background, showing remarkable potential for anti-counterfeit techniques. Besides, we demonstrate that SAPCs yield different RGB histograms that depend on viewing angles and pattern densities, thus enhancing their cryptographic capabilities. Hence, the structural colorations designed by inkjet printers would not only produce optical holograms for the simple authentication of many items and products but also enable a high-secure anti-counterfeit technique.

Growth and characterization of 4-chloro-3-nitrobenzophenone single crystals using vertical Bridgman technique

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

Aravinth, K., E-mail: anandcgc@gmail.com; Babu, G. Anandha, E-mail: anandcgc@gmail.com; Ramasamy, P., E-mail: anandcgc@gmail.com

2014-04-24

4-chloro-3-nitrobenzophenone (4C3N) has been grown by using vertical Bridgman technique. The grown crystal was confirmed by Powder X-ray diffraction analysis. The crystalline perfection of the grown crystal was examined by high-resolution X-ray diffraction study. The fluorescence spectra of grown 4C3N single crystals exhibit emission peak at 575 nm. The micro hardness measurements were used to analyze the mechanical property of the grown crystal.

Sparsity-based image monitoring of crystal size distribution during crystallization

NASA Astrophysics Data System (ADS)

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

2017-07-01

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

Peculiar orientational disorder in 4-bromo-4'-nitrobiphenyl (BNBP) and 4-bromo-4'-cyanobiphenyl (BCNBP) leading to bipolar crystals.

PubMed

Burgener, Matthias; Aboulfadl, Hanane; Labat, Gaël Charles; Bonin, Michel; Sommer, Martin; Sankolli, Ravish; Wübbenhorst, Michael; Hulliger, Jürg

2016-05-01

180° orientational disorder of molecular building blocks can lead to a peculiar spatial distribution of polar properties in molecular crystals. Here we present two examples [4-bromo-4'-nitrobiphenyl (BNBP) and 4-bromo-4'-cyanobiphenyl (BCNBP)] which develop into a bipolar final growth state. This means orientational disorder taking place at the crystal/nutrient interface produces domains of opposite average polarity for as-grown crystals. The spatial inhomogeneous distribution of polarity was investigated by scanning pyroelectric microscopy (SPEM), phase-sensitive second harmonic microscopy (PS-SHM) and selected volume X-ray diffraction (SVXD). As a result, the acceptor groups (NO2 or CN) are predominantly present at crystal surfaces. However, the stochastic process of polarity formation can be influenced by adding a symmetrical biphenyl to a growing system. For this case, Monte Carlo simulations predict an inverted net polarity compared with the growth of pure BNBP and BCNBP. SPEM results clearly demonstrate that 4,4'-dibromobiphenyl (DBBP) can invert the polarity for both crystals. Phenomena reported in this paper belong to the most striking processes seen for molecular crystals, demonstrated by a stochastic process giving rise to symmetry breaking. We encounter here further examples supporting the general thesis that monodomain polar molecular crystals for fundamental reasons cannot exist.

Crystal growth and characterization of third order nonlinear optical piperazinium bis(4-hydroxybenzenesulphonate) (P4HBS) single crystal

NASA Astrophysics Data System (ADS)

Pichan, Karuppasamy; Muthu, Senthil Pandian; Perumalsamy, Ramasamy

2017-09-01

The organic single crystal of piperazinium bis(4-hydroxybenzenesulphonate) (P4HBS) was grown by slow evaporation solution technique (SEST) at room temperature. The lattice parameters of the grown crystal were confirmed by single crystal X-ray diffraction analysis. Functional groups of P4HBS crystal were confirmed by FTIR spectrum analysis. The optical quality of the grown crystal was identified by the UV-Vis NIR spectrum analysis. The grown crystal has good optical transmittance in the range of 410-1100 nm. In photoluminescence spectrum, sharp emission peaks are observed, which indicates the ultraviolet (UV) emission. The photoconductivity study reveals that the grown crystal has negative photoconductive nature. The thermal behaviour of the P4HBS crystal was investigated by thermogravimetric and differential thermal analysis (TG-DTA). The mechanical stability of grown crystal was analyzed and the indentation size effect (ISE) was explained by Hays-Kendall's (HK) approach and proportional specimen resistance model (PSRM). Chemical etching study was carried out and the etch pit density (EPD) was calculated. The dielectric constant (ε‧) and dielectric loss (tan δ) as a function of frequency were measured for the grown crystal. The solid state parameters such as valence electron, plasma energy, Penn gap and Fermi energy were evaluated theoretically for the P4HBS using the empirical relation. The estimated values are used to calculate the electronic polarizability. 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 632.8 nm using He-Ne laser.

Development of ^{100}Mo-containing scintillating bolometers for a high-sensitivity neutrinoless double-beta decay search

NASA Astrophysics Data System (ADS)

Armengaud, E.; Augier, C.; Barabash, A. S.; Beeman, J. W.; Bekker, T. B.; Bellini, F.; Benoît, A.; Bergé, L.; Bergmann, T.; Billard, J.; Boiko, R. S.; Broniatowski, A.; Brudanin, V.; Camus, P.; Capelli, S.; Cardani, L.; Casali, N.; Cazes, A.; Chapellier, M.; Charlieux, F.; Chernyak, D. M.; de Combarieu, M.; Coron, N.; Danevich, F. A.; Dafinei, I.; Jesus, M. De; Devoyon, L.; Domizio, S. Di; Dumoulin, L.; Eitel, K.; Enss, C.; Ferroni, F.; Fleischmann, A.; Foerster, N.; Gascon, J.; Gastaldo, L.; Gironi, L.; Giuliani, A.; Grigorieva, V. D.; Gros, M.; Hehn, L.; Hervé, S.; Humbert, V.; Ivannikova, N. V.; Ivanov, I. M.; Jin, Y.; Juillard, A.; Kleifges, M.; Kobychev, V. V.; Konovalov, S. I.; Koskas, F.; Kozlov, V.; Kraus, H.; Kudryavtsev, V. A.; Laubenstein, M.; Sueur, H. Le; Loidl, M.; Magnier, P.; Makarov, E. P.; Mancuso, M.; de Marcillac, P.; Marnieros, S.; Marrache-Kikuchi, C.; Nagorny, S.; Navick, X.-F.; Nikolaichuk, M. O.; Nones, C.; Novati, V.; Olivieri, E.; Pagnanini, L.; Pari, P.; Pattavina, L.; Pavan, M.; Paul, B.; Penichot, Y.; Pessina, G.; Piperno, G.; Pirro, S.; Plantevin, O.; Poda, D. V.; Queguiner, E.; Redon, T.; Rodrigues, M.; Rozov, S.; Rusconi, C.; Sanglard, V.; Schäffner, K.; Scorza, S.; Shlegel, V. N.; Siebenborn, B.; Strazzer, O.; Tcherniakhovski, D.; Tomei, C.; Tretyak, V. I.; Umatov, V. I.; Vagneron, L.; Vasiliev, Ya. V.; Velázquez, M.; Vignati, M.; Weber, M.; Yakushev, E.; Zolotarova, A. S.

2017-11-01

This paper reports on the development of a technology involving ^{100}Mo-enriched scintillating bolometers, compatible with the goals of CUPID, a proposed next-generation bolometric experiment to search for neutrinoless double-beta decay. Large mass (˜ 1 kg), high optical quality, radiopure ^{100}Mo-containing zinc and lithium molybdate crystals have been produced and used to develop high performance single detector modules based on 0.2-0.4 kg scintillating bolometers. In particular, the energy resolution of the lithium molybdate detectors near the Q-value of the double-beta transition of ^{100}Mo (3034 keV) is 4-6 keV FWHM. The rejection of the α -induced dominant background above 2.6 MeV is better than 8σ . Less than 10 μ Bq/kg activity of ^{232}Th (^{228}Th) and ^{226}Ra in the crystals is ensured by boule recrystallization. The potential of ^{100}Mo-enriched scintillating bolometers to perform high sensitivity double-beta decay searches has been demonstrated with only 10 kg× d exposure: the two neutrino double-beta decay half-life of ^{100}Mo has been measured with the up-to-date highest accuracy as T_{1/2} = [6.90 ± 0.15(stat.) ± 0.37(syst.)] × 10^{18} years. Both crystallization and detector technologies favor lithium molybdate, which has been selected for the ongoing construction of the CUPID-0/Mo demonstrator, containing several kg of ^{100}Mo.

Efficient continuous-wave and passively Q-switched pulse laser operations in a diffusion-bonded sapphire/Er:Yb:YAl3(BO3)4/sapphire composite crystal around 1.55 μm.

PubMed

Chen, Yujin; Lin, Yanfu; Huang, Jianhua; Gong, Xinghong; Luo, Zundu; Huang, Yidong

2018-01-08

A composite crystal consisting of a 1.5-mm-thick Er:Yb:YAl 3 (BO 3 ) 4 crystal between two 1.2-mm-thick sapphire crystals was fabricated by the thermal diffusion bonding technique. Compared with a lone Er:Yb:YAl 3 (BO 3 ) 4 crystal measured under the identical experimental conditions, higher laser performances were demonstrated in the sapphire/Er:Yb:YAl 3 (BO 3 ) 4 /sapphire composite crystal due to the reduction of the thermal effects. End-pumped by a 976 nm laser diode in a hemispherical cavity, a 1.55 μm continuous-wave laser with a maximum output power of 1.75 W and a slope efficiency of 36% was obtained in the composite crystal when the incident pump power was 6.54 W. Passively Q-switched by a Co 2+ :MgAl 2 O 4 crystal, a 1.52 μm pulse laser with energy of 10 μJ and repetition frequency of 105 kHz was also realized in the composite crystal. Pulse width was 315 ns. The results show that the sapphire/Er:Yb:YAl 3 (BO 3 ) 4 /sapphire composite crystal is an excellent active element for 1.55 μm laser.

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.

A simple 2D composite image analysis technique for the crystal growth study of L-ascorbic acid.

PubMed

Kumar, Krishan; Kumar, Virender; Lal, Jatin; Kaur, Harmeet; Singh, Jasbir

2017-06-01

This work was destined for 2D crystal growth studies of L-ascorbic acid using the composite image analysis technique. Growth experiments on the L-ascorbic acid crystals were carried out by standard (optical) microscopy, laser diffraction analysis, and composite image analysis. For image analysis, the growth of L-ascorbic acid crystals was captured as digital 2D RGB images, which were then processed to composite images. After processing, the crystal boundaries emerged as white lines against the black (cancelled) background. The crystal boundaries were well differentiated by peaks in the intensity graphs generated for the composite images. The lengths of crystal boundaries measured from the intensity graphs of composite images were in good agreement (correlation coefficient "r" = 0.99) with the lengths measured by standard microscopy. On the contrary, the lengths measured by laser diffraction were poorly correlated with both techniques. Therefore, the composite image analysis can replace the standard microscopy technique for the crystal growth studies of L-ascorbic acid. © 2017 Wiley Periodicals, Inc.

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

PubMed

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

2006-07-06

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

Numerical modeling of Czochralski growth of Li2MoO4 crystals for heat-scintillation cryogenic bolometers

NASA Astrophysics Data System (ADS)

Stelian, Carmen; Velázquez, Matias; Veber, Philippe; Ahmine, Abdelmounaim; Sand, Jean-Baptiste; Buşe, Gabriel; Cabane, Hugues; Duffar, Thierry

2018-06-01

Lithium molybdate Li2MoO4 (LMO) crystals of mass ranging between 350 and 500 g are excellent candidates to build heat-scintillation cryogenic bolometers likely to be used for the detection of rare events in astroparticle physics. In this work, numerical modeling is applied in order to investigate the Czochralski growth of Li2MoO4 crystals in an inductive furnace. The numerical model was validated by comparing the numerical predictions of the crystal-melt interface shape to experimental visualization of the growth interface. Modeling was performed for two different Czochralski furnaces that use inductive heating. The simulation of the first furnace, which was used to grow Li2MoO4 crystals of 3-4 cm in diameter, reveals non-optimal heat transfer conditions for obtaining good quality crystals. The second furnace, which will be used to grow crystals of 5 cm in diameter, was numerically optimized in order to reduce the temperature gradients in the crystal and to avoid fast crystallization of the bath at the later stages of the growth process.

An evaluation of adhesive sample holders for advanced crystallographic experiments

PubMed Central

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

2014-01-01

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

The calorimeter of the Mu2e experiment at Fermilab

DOE PAGES

Atanov, N.; Baranov, V.; Budagov, J.; ...

2017-01-23

Here, the Mu2e experiment at Fermilab looks for Charged Lepton Flavor Violation (CLFV) improving by 4 orders of magnitude the current experimental sensitivity for the muon to electron conversion in a muonic atom. A positive signal could not be explained in the framework of the current Standard Model of particle interactions and therefore would be a clear indication of new physics. In 3 years of data taking, Mu2e is expected to observe less than one background event mimicking the electron coming from muon conversion. Achieving such a level of background suppression requires a deep knowledge of the experimental apparatus: amore » straw tube tracker, measuring the electron momentum and time, a cosmic ray veto system rejecting most of cosmic ray background and a pure CsI crystal calorimeter, that will measure time of flight, energy and impact position of the converted electron. The calorimeter has to operate in a harsh radiation environment, in a 10 -4 Torr vacuum and inside a 1 T magnetic field. The results of the first qualification tests of the calorimeter components are reported together with the energy and time performances expected from the simulation and measured in beam tests of a small scale prototype.« less

Plastically bendable crystals of probenecid and its cocrystal with 4,4‧-Bipyridine

NASA Astrophysics Data System (ADS)

Nath, Naba K.; Hazarika, Mousumi; Gupta, Poonam; Ray, Nisha R.; Paul, Amit K.; Nauha, Elisa

2018-05-01

Recent findings of plastically bendable molecular crystals led to the realization that design based strategies are required for these materials to be useful in real life application. We have coincidentally discovered plastically bendable crystals of a drug molecule probenecid. Based on the structural features of its crystals at room temperature, we hypothesized that introduction of a molecular spacer between two hydrogen bonded molecules of probenecid, by replacing the carboxylic acid homodimer with similar dimeric hydrogen bonding synthon, would not disturb the layered molecular packing of probenecid. As a consequence, the new multi-component crystal would retain flexibility similar to the original probenecid crystals. Herein we have attempted to prove this hypothesis and we were successful in the case of probenecid: 4,4‧-bipyridine cocrystal. As designed, in the crystal structure 4,4‧-bypyridine molecule acted as spacer and connected two probenecid molecules resulting in the retention of the slip planes which are necessary for a molecular crystal to be plastically bendable. DFT computational calculations were carried out to account for the hydrogen bonding synthons between probenecid and the coformers under study.

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

PubMed Central

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

2015-01-01

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

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

PubMed

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

2015-10-01

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

Crystallization pathways of sulfate-nitrate-ammonium aerosol particles.

PubMed

Schlenker, Julie C; Martin, Scot T

2005-11-10

Crystallization experiments are conducted for aerosol particles composed of aqueous mixtures of (NH(4))(2)SO(4)(aq) and NH(4)NO(3)(aq), (NH(4))(2)SO(4)(aq) and NH(4)HSO(4)(aq), and NH(4)NO(3)(aq) and NH(4)HSO(4)(aq). Depending on the aqueous composition, crystals of (NH(4))(2)SO(4)(s), (NH(4))(3)H(SO(4))(2)(s), NH(4)HSO(4)(s), NH(4)NO(3)(s), 2NH(4)NO(3) x (NH(4))(2)SO(4)(s), and 3NH(4)NO(3) x (NH(4))(2)SO(4)(s) are formed. Although particles of NH(4)NO(3)(aq) and NH(4)HSO(4)(aq) do not crystallize even at 1% relative humidity, additions of 0.05 mol fraction SO(4)(2-)(aq) or NO(3)(-)(aq) ions promote crystallization, respectively. 2NH(4)NO(3) x (NH(4))(2)SO(4)(s) and (NH(4))(3)H(SO(4))(2)(s) appear to serve as good heterogeneous nuclei for NH(4)NO(3)(s) and NH(4)HSO(4)(s), respectively. 2NH(4)NO(3) x (NH(4))(2)SO(4)(s) crystallizes over a greater range of aqueous compositions than 3NH(4)NO(3) x (NH(4))(2)SO(4)(s). An infrared aerosol spectrum is provided for each solid based upon a linear decomposition analysis of the recorded spectra. Small nonzero residuals occur in the analysis because aerosol spectra depend on particle morphology, which changes slightly across the range of compositions studied. In addition, several of the mixed compositions crystallize with residual aqueous water of up to 5% particle mass. We attribute this water content to enclosed water pockets. The results provide further insights into the nonlinear crystallization pathways of sulfate-nitrate-ammonium aerosol particles.

Synthesis and structural study of 4-(2-chlorophenyl)-2-ethoxy-5,6,7,8,9,10-hexahydrocycloocta[B]pyridine-3-carbonitrile

NASA Astrophysics Data System (ADS)

Fathima, K. Saiadali; Vasumathi, M.; Anitha, K.

2016-05-01

The novel organic material C20H21ClN2O was synthesized by One-Pot synthesis method and the single crystals were grown by slow evaporation solution growth technique. The crystal structure was elucidated by subjecting the grown crystals to the single crystal x-ray diffraction analysis and was refined by full matrix least-squares method to R=0.039 for 2746 reflections. Crystal system of the grown crystal was found to be monoclinic with the space group P21/a and a=9.196(4) Å, b=13.449(4) Å, c=14.818(4) Å, β= 101.542(3)°, V=1795.6(11) Å3 and Z=4. In this crystal structure, cyclooctanone prefers to reside in a chair-boat conformation. The structure is stabilized by attractive molecular force such as CH/π interaction called hydrophobic interaction.

Double-beta decay investigation with highly pure enriched $$^{82}$$Se for the LUCIFER experiment

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

Beeman, J. W.; Bellini, F.; Benetti, P.

2015-12-13

The LUCIFER project aims at deploying the first array of enriched scintillating bolometers for the investigation of neutrinoless double-beta decay of 82Se. The matrix which embeds the source is an array of ZnSe crystals, where enriched 82Se is used as decay isotope. The radiopurity of the initial components employed for manufacturing crystals, that can be operated as bolometers, is crucial for achieving a null background level in the region of interest for double-beta decay investigations. In this work, we evaluated the radioactive content in 2.5 kg of 96.3 % enriched 82Se metal, measured with a high-purity germanium detector at themore » Gran Sasso deep underground laboratory. The limits on internal contaminations of primordial decay chain elements of 232Th, 238U and 235U are respectively: <61, <110 and <74 μBq/kg at 90 % C.L. The extremely low-background conditions in which the measurement was carried out and the high radiopurity of the 82Se allowed us to establish the most stringent lower limits on the half-lives of the double-beta decay of 82Se to 0+1, 2+2 and 2+1 excited states of 82Kr of 3.4•10 22, 1.3•10 22 and 1.0•10 22 y, respectively, with a 90 % C.L.« less

Bulk growth of <001> organic nonlinear optical (NLO) L-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) single crystals by SR method

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

Pandian, Muthu Senthil, E-mail: senthilpandianm@ssn.edu.in; Sivasubramani, V.; Ramasamy, P.

2015-06-24

A transparent uniaxial L-arginine 4-nitrophenolate 4-nitrophenol dehydrate (LAPP) single crystal having dimension of 20 mm diameter and 45 mm length was grown by Sankaranarayanan-Ramasamy (SR) method with a growth rate of 1 mm per day. Using an identical solution the conventional crystal grown to a dimension of 8×5×5 mm{sup 3} was obtained over a period of 30 days. The crystal structure has been confirmed by single crystal X-ray diffraction measurement. The crystalline perfection of LAPP crystals grown by slow evaporation solution technique (SEST) and SR method were characterized using Vickers microhardness, UV-Vis NIR, chemical etching, dark and photo current measurements. The above study indicatesmore » that the crystal quality of the Sankaranarayanan-Ramasamy (SR) method grown LAPP is good compared to the conventional method grown 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.

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.

The Biomolecular Crystallization Database Version 4: expanded content and new features.

PubMed

Tung, Michael; Gallagher, D Travis

2009-01-01

The Biological Macromolecular Crystallization Database (BMCD) has been a publicly available resource since 1988, providing a curated archive of information on crystal growth for proteins and other biological macromolecules. The BMCD content has recently been expanded to include 14 372 crystal entries. The resource continues to be freely available at http://xpdb.nist.gov:8060/BMCD4. In addition, the software has been adapted to support the Java-based Lucene query language, enabling detailed searching over specific parameters, and explicit search of parameter ranges is offered for five numeric variables. Extensive tools have been developed for import and handling of data from the RCSB Protein Data Bank. The updated BMCD is called version 4.02 or BMCD4. BMCD4 entries have been expanded to include macromolecule sequence, enabling more elaborate analysis of relations among protein properties, crystal-growth conditions and the geometric and diffraction properties of the crystals. The BMCD version 4.02 contains greatly expanded content and enhanced search capabilities to facilitate scientific analysis and design of crystal-growth strategies.

Probing the crystal structure landscape by doping: 4-bromo, 4-chloro and 4-methylcinnamic acids.

PubMed

Desiraju, Gautam R; Chakraborty, Shaunak; Joseph, Sumy

2018-06-11

Accessing the data points in the crystal structure landscape of a molecule is a challenging task, either experimentally or computationally. We have charted the crystal structure landscape of 4-bromocinnamic acid (4BCA) experimentally and computationally: experimental doping is achieved with 4-methylcinnamic acid (4MCA) to obtain new crystal structures; computational doping is performed with 4-chlorocinnamic acid (4CCA) as a model system, because of the difficulties associated in parameterizing the Br-atom. The landscape of 4CCA is explored experimentally in turn, also by doping it with 4MCA, and is found to bear a close resemblance to the landscape of 4BCA, justifying the ready miscibility of these two halogenated cinnamic acids to form solid solutions without any change in crystal structure. In effect, 4MCA, 4CCA and 4BCA form a commutable group of crystal structures, which may be realized experimentally or computationally, and constitute the landscape. Unlike the results obtained by Kitaigorodskii and others, all but two of the multiple solid solutions obtained in the methyl-doping experiments take structures that are different from the hitherto observed crystal forms of the parent compounds. Even granted that the latter might be inherently polymorphic, this unusual observation provokes the suggestion that solid solution formation may be used to probe the crystal structure landscape. The influence of pi...pi interactions, weak hydrogen bonds and halogen bonds in directing the formation of these new structures is also seen. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Production of low-background CuSn6-bronze for the CRESST dark-matter-search experiment.

PubMed

Majorovits, B; Kader, H; Kraus, H; Lossin, A; Pantic, E; Petricca, F; Proebst, F; Seidel, W

2009-01-01

One of the most intriguing open questions in modern particle physics is the nature of the dark matter in our universe. As hypothetical weakly interacting massive particles (WIMPs) do interact with ordinary matter extremely rarely, their observation requires a very low-background detector environment regarding radioactivity as well as an advanced detector technique that allows for active discrimination of the still present radioactive contaminations. The CRESST experiment uses detectors operating at milli-Kelvin temperature. Energy deposition in the detectors is recorded via the simultaneous measurement of a phonon-mediated signal and scintillation emitted by the CaWO(4) crystal targets. The entire setup is made of carefully selected materials. In this note we report on the development of ultra-pure bronze (CuSn(6)) wire in small quantities for springs and clamps that are currently being used in the CRESST II setup.

Self-powdering and nonlinear optical domain structures in ferroelastic β‧-Gd2(MoO4)3 crystals formed in glass

NASA Astrophysics Data System (ADS)

Tsukada, Y.; Honma, T.; Komatsu, T.

2009-08-01

Ferroelastic β'-Gd 2(MoO 4) 3, (GMO), crystals are formed through the crystallization of 21.25Gd 2O 3-63.75MoO 3-15B 2O 3 glass (mol%), and two scientific curious phenomena are observed. (1) GMO crystals formed in the crystallization break into small pieces with a triangular prism or pyramid shape having a length of 50-500 μm spontaneously during the crystallizations in the inside of an electric furnace, not during the cooling in air after the crystallization. This phenomenon is called "self-powdering phenomenon during crystallization" in this paper. (2) Each self-powdered GMO crystal grain shows a periodic domain structure with different refractive indices, and a spatially periodic second harmonic generation (SHG) depending on the domain structure is observed. It is proposed from polarized micro-Raman scattering spectra and the azimuthal dependence of second harmonic intensities that GMO crystals are oriented in each crystal grain and the orientation of (MoO 4) 2- tetrahedra in GMO crystals changes periodically due to spontaneous strains in ferroelastic GMO crystals.

Growth, Crystal Structure and Magnetic Characterization of Zn-Stabilized CePtIn4

NASA Astrophysics Data System (ADS)

Carnicom, Elizabeth M.; Klimczuk, Tomasz; von Rohr, Fabian; Winiarski, Michal J.; Kong, Tai; Stolze, Karoline; Xie, Weiwei; Kushwaha, Satya K.; Cava, Robert J.

2017-08-01

The growth and characterization of CePtIn4, stabilized by 10% Zn substitution for In, is reported. The new material is orthorhombic, space group Cmcm (No. 63), with lattice parameters a = 4.51751(4) Å, b = 16.7570(2) Å, and c = 7.36682(8) Å, and the refined crystal composition has 10% of Zn substituted for In, i.e., the crystals are CePt(In0.9Zn0.1)4. Crystals were grown using a self-flux method: only growths containing Zn yielded CePtIn4 crystals, while Ce3Pt4In13 crystals formed when Zn was not present. Anisotropic temperature-dependent magnetic susceptibilities for single crystals show that Zn-stabilized CePtIn4 orders magnetically at ˜1.9 K. High-temperature Curie-Weiss fits indicate an effective moment of ˜2.49 μB/Ce and a directionally averaged Weiss-temperature of approximately -31 K. Specific heat data shows a peak consistent with the ordering temperature seen in the magnetic susceptibility data. Zn-stabilized CePtIn4 is metallic and displays no superconducting transition down to 0.14 K.

First search for a dark matter annual modulation signal with NaI(Tl) in the Southern Hemisphere by DM-Ice17

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

Barbosa de Souza, E.; Cherwinka, J.; Cole, A.

The first search for a dark matter annual modulation signal with NaI(Tl) target material in the Southern Hemisphere conducted with the DM-Ice17 experiment is presented. DM-Ice17 consists of 17 kg of NaI(Tl) scintillating crystal under 2200 m.w.e. overburden of Antarctic glacial ice. The analysis presented here utilizes a 60.8 kg yr exposure. While unable to exclude the signal reported by DAMA/LIBRA, the DM-Ice17 data are consistent with no modulation in the energy range of 4-20 keV, providing the strongest limits on WIMP candidates from a direct detection experiment located in the Southern Hemisphere. Additionally, the successful deployment and stable operationmore » of 17 kg of NaI(Tl) crystal over 3.5 years establishes the South Pole ice as a viable location for future underground, low-background experiments.« less

Bridgman growth and scintillation properties of calcium tungstate single crystal

NASA Astrophysics Data System (ADS)

Wang, Zhenhai; Jiang, Linwen; Chen, Yaping; Chen, Peng; Chen, Hongbing; Mao, Rihua

2017-12-01

CaWO4 single crystal with large size was grown by Bridgman method. The results of transmission spectra show that the transmittance of CaWO4 crystal reaches 79-85% in 320-800 nm wavelength range. The refraction index is near 1.80 in visible and infrared region. CaWO4 crystal shows a broad emission band centered at 424 nm under X-ray excitation and centered at 416 nm under ultraviolet (λex = 280 nm) excitation. The decay kinetics of CaWO4 single crystal shows double-exponential decay with fast decay constant τ1 = 5.4 μs and slow decay constant τ2 = 177.1 μs. The energy resolution of CaWO4 crystal was found to be 31.6% in the net peak of 545.9 channel. Meanwhile, the absolute output is at the lever of 19,000 ± 1000 photons/MeV. The results indicate the scintillator of CaWO4 single crystal has great potential in the applications of high-energy physics and nuclear physics due to its high light output and great energy resolution.

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

Stauber, Mark; Yeshiva University, 2495 Amsterdam Avenue, New York, NY 10033-3312; Jakoncic, Jean

Crystallization of lysozyme with (R)-2-methyl-2, 4-pentanediol produces more ordered crystals and a higher resolution protein structure than crystallization with (S)-2-methyl-2, 4-pentanediol. The results suggest that chiral interactions with chiral additives are important in protein crystal formation. Chiral control of crystallization has ample precedent in the small-molecule world, but relatively little is known about the role of chirality in protein crystallization. In this study, lysozyme was crystallized in the presence of the chiral additive 2-methyl-2, 4-pentanediol (MPD) separately using the R and S enantiomers as well as with a racemic RS mixture. Crystals grown with (R)-MPD had the most order andmore » produced the highest resolution protein structures. This result is consistent with the observation that in the crystals grown with (R)-MPD and (RS)-MPD the crystal contacts are made by (R)-MPD, demonstrating that there is preferential interaction between lysozyme and this enantiomer. These findings suggest that chiral interactions are important in protein crystallization.« less

Thermal evolution of old white dwarfs

NASA Astrophysics Data System (ADS)

Kozhberov, Andrew

2017-11-01

This work is devoted to a description of thermodynamic properties of Coulomb crystals which are expected to form in white dwarf interiors. Effects of magnetic field, isotopic impurities, polarization of the electron background and crystal lattice type on the thermal evolution of white dwarfs are discussed. It is shown that the electron polarization could play a noticeable role in the cooling process. While other parameters in concern do not make a significant impact.

Lensing effects in a nematic liquid crystal with topological defects.

PubMed

Sátiro, C; Moraes, F

2006-06-01

Light traveling through a liquid crystal with disclinations perceives a geometrical background which causes lensing effects similar to the ones predicted for cosmic objects like global monopoles and cosmic strings. In this paper we explore the effective geometry as perceived by light in such media. The comparison between both systems suggests that experiments can be done in the laboratory to simulate optical properties, like gravitational lensing, of cosmic objects.

STS-57 Commander Grabe adjusts Thermal Enclosure System (TES) aboard OV-105

NASA Technical Reports Server (NTRS)

1993-01-01

STS-57 Commander Ronald J. Grabe adjusts a bolt on the Thermal Enclosure System (TES) with Crystal Observation System (COS) experiment installation located in an aft locker (MA16J) on the middeck of Endeavour, Orbiter Vehicle (OV) 105. Holding a camcorder in his right hand, Grabe prepares to monitor and record the crystal growth. The open airlock hatch is partially visible in the background.

Naturally occurring 32Si and low-background silicon dark matter detectors

DOE PAGES

Orrell, John L.; Arnquist, Isaac J.; Bliss, Mary; ...

2018-02-10

Here, the naturally occurring radioisotope 32Si represents a potentially limiting background in future dark matter direct-detection experiments. We investigate sources of 32Si and the vectors by which it comes to reside in silicon crystals used for fabrication of radiation detectors. We infer that the 32Si concentration in commercial single-crystal silicon is likely variable, dependent upon the specific geologic and hydrologic history of the source (or sources) of silicon “ore” and the details of the silicon-refinement process. The silicon production industry is large, highly segmented by refining step, and multifaceted in terms of final product type, from which we conclude thatmore » production of 32Si-mitigated crystals requires both targeted silicon material selection and a dedicated refinement-through-crystal-production process. We review options for source material selection, including quartz from an underground source and silicon isotopically reduced in 32Si. To quantitatively evaluate the 32Si content in silicon metal and precursor materials, we propose analytic methods employing chemical processing and radiometric measurements. Ultimately, it appears feasible to produce silicon detectors with low levels of 32Si, though significant assay method development is required to validate this claim and thereby enable a quality assurance program during an actual controlled silicon-detector production cycle.« less

Naturally occurring 32Si and low-background silicon dark matter detectors

NASA Astrophysics Data System (ADS)

Orrell, John L.; Arnquist, Isaac J.; Bliss, Mary; Bunker, Raymond; Finch, Zachary S.

2018-05-01

The naturally occurring radioisotope 32Si represents a potentially limiting background in future dark matter direct-detection experiments. We investigate sources of 32Si and the vectors by which it comes to reside in silicon crystals used for fabrication of radiation detectors. We infer that the 32Si concentration in commercial single-crystal silicon is likely variable, dependent upon the specific geologic and hydrologic history of the source (or sources) of silicon "ore" and the details of the silicon-refinement process. The silicon production industry is large, highly segmented by refining step, and multifaceted in terms of final product type, from which we conclude that production of 32Si-mitigated crystals requires both targeted silicon material selection and a dedicated refinement-through-crystal-production process. We review options for source material selection, including quartz from an underground source and silicon isotopically reduced in 32Si. To quantitatively evaluate the 32Si content in silicon metal and precursor materials, we propose analytic methods employing chemical processing and radiometric measurements. Ultimately, it appears feasible to produce silicon detectors with low levels of 32Si, though significant assay method development is required to validate this claim and thereby enable a quality assurance program during an actual controlled silicon-detector production cycle.

Raster-scanning serial protein crystallography using micro- and nano-focused synchrotron beams

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

Coquelle, Nicolas; CNRS, IBS, 38044 Grenoble; CEA, IBS, 38044 Grenoble

A raster scanning serial protein crystallography approach is presented, that consumes as low ∼200–700 nl of sedimented crystals. New serial data pre-analysis software, NanoPeakCell, is introduced. High-resolution structural information was obtained from lysozyme microcrystals (20 µm in the largest dimension) using raster-scanning serial protein crystallography on micro- and nano-focused beamlines at the ESRF. Data were collected at room temperature (RT) from crystals sandwiched between two silicon nitride wafers, thereby preventing their drying, while limiting background scattering and sample consumption. In order to identify crystal hits, new multi-processing and GUI-driven Python-based pre-analysis software was developed, named NanoPeakCell, that was able tomore » read data from a variety of crystallographic image formats. Further data processing was carried out using CrystFEL, and the resultant structures were refined to 1.7 Å resolution. The data demonstrate the feasibility of RT raster-scanning serial micro- and nano-protein crystallography at synchrotrons and validate it as an alternative approach for the collection of high-resolution structural data from micro-sized crystals. Advantages of the proposed approach are its thriftiness, its handling-free nature, the reduced amount of sample required, the adjustable hit rate, the high indexing rate and the minimization of background scattering.« less

Naturally occurring 32Si and low-background silicon dark matter detectors

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

Orrell, John L.; Arnquist, Isaac J.; Bliss, Mary

Here, the naturally occurring radioisotope 32Si represents a potentially limiting background in future dark matter direct-detection experiments. We investigate sources of 32Si and the vectors by which it comes to reside in silicon crystals used for fabrication of radiation detectors. We infer that the 32Si concentration in commercial single-crystal silicon is likely variable, dependent upon the specific geologic and hydrologic history of the source (or sources) of silicon “ore” and the details of the silicon-refinement process. The silicon production industry is large, highly segmented by refining step, and multifaceted in terms of final product type, from which we conclude thatmore » production of 32Si-mitigated crystals requires both targeted silicon material selection and a dedicated refinement-through-crystal-production process. We review options for source material selection, including quartz from an underground source and silicon isotopically reduced in 32Si. To quantitatively evaluate the 32Si content in silicon metal and precursor materials, we propose analytic methods employing chemical processing and radiometric measurements. Ultimately, it appears feasible to produce silicon detectors with low levels of 32Si, though significant assay method development is required to validate this claim and thereby enable a quality assurance program during an actual controlled silicon-detector production cycle.« less

Naturally occurring 32 Si and low-background silicon dark matter detectors

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

Orrell, John L.; Arnquist, Isaac J.; Bliss, Mary

The naturally occurring radioisotope Si-32 represents a potentially limiting background in future dark matter direct-detection experiments. We investigate sources of Si-32 and the vectors by which it comes to reside in silicon crystals used for fabrication of radiation detectors. We infer that the Si-32 concentration in commercial single-crystal silicon is likely variable, dependent upon the specific geologic and hydrologic history of the source (or sources) of silicon “ore” and the details of the silicon-refinement process. The silicon production industry is large, highly segmented by refining step, and multifaceted in terms of final product type, from which we conclude that productionmore » of Si-32-mitigated crystals requires both targeted silicon material selection and a dedicated refinement-through-crystal-production process. We review options for source material selection, including quartz from an underground source and silicon isotopically reduced in Si-32. To quantitatively evaluate the Si-32 content in silicon metal and precursor materials, we propose analytic methods employing chemical processing and radiometric measurements. Ultimately, it appears feasible to produce silicon-based detectors with low levels of Si-32, though significant assay method development is required to validate this claim and thereby enable a quality assurance program during an actual controlled silicon-detector production cycle.« less

Dielectric constant adjustments in computations of the scattering properties of solid ice crystals using the Generalized Multi-particle Mie method

NASA Astrophysics Data System (ADS)

Lu, Yinghui; Aydin, Kültegin; Clothiaux, Eugene E.; Verlinde, Johannes

2014-03-01

Ice crystal scattering properties at microwave radar wavelengths can be modeled with the Generalized Multi-particle Mie (GMM) method by decomposing an ice crystal into a cluster of tiny spheres composed of solid ice. In this decomposition the mass distribution of the tiny spheres in the cluster is no longer equivalent to that in the original ice crystal because of gaps between the tiny spheres. To compensate for the gaps in the cluster representation of an ice crystal in the GMM computation of crystal scattering properties, the Maxwell Garnett approximation is used to estimate what the dielectric function of the tiny spheres (i.e., the inclusions) in the cluster must be to make the cluster of tiny spheres with associated air gaps (i.e., the background matrix) dielectrically equivalent to the original solid ice crystal. Overall, compared with the T-matrix method for spheroids outside resonance regions this approach agrees to within mostly 0.3 dB (and often better) in the horizontal backscattering cross section σhh and the ratio of horizontal and vertical backscattering cross sections σhh/σvv, and 6% for the amplitude scattering matrix elements Re{S22-S11} and Im{S22} in the forward direction. For crystal sizes and wavelengths near resonances, where the scattering parameters are highly sensitive to the crystal shape, the differences are generally within 1.2 dB for σhh and σhh/σvv, 20% for Re{S22-S11} and 6% for Im{S22}. The Discrete Dipole Approximation (DDA) results for the same spheroids are generally closer than those of GMM to the T-matrix results. For hexagonal plates the differences between GMM and the DDA at a W-band wavelength (3.19 mm) are mostly within 0.6 dB for σhh, 1 dB for σhh/σvv, 11% for Re{S22-S11} and 12% for Im{S22}. For columns the differences are within 0.3 dB for σhh and σhh/σvv, 8% for Re{S22-S11} and 4% for Im{S22}. This method shows higher accuracy than an alternative method that artificially increases the thickness of ice plates to provide the same mass as the original ice crystal.

In Situ High Temperature High Pressure MAS NMR Study on the Crystallization of AlPO 4 -5

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

Zhao, Zhenchao; Xu, Suochang; Hu, Mary Y.

2016-01-28

A damped oscillating crystallization process of AlPO4-5 at the presence of small amount of water is demonstrated by in situ high temperature high pressure multinuclear MAS NMR. Crystalline AlPO4-5 is formed from an intermediate semicrystalline phase via continuous rearrangement of the local structure of amorphous precursor gel. Activated water catalyzes the rearrangement via repeatedly hydrolysis and condensation reaction. Strong interactions between organic template and inorganic species facilitate the ordered rearrangement. During the crystallization process, excess water, phosphate, and aluminums are expelled from the precursor. The oscillating crystallization reflects mass transportation between the solid and liquid phase during the crystallization process.more » This crystallization process is also applicable to AlPO4-5 crystallized in the presence of a relatively large amount of water.« less

Crystal structure, Raman scattering and magnetic properties of CuCr2-xZrxSe4 and CuCr2-xSnxSe4 selenospinels

NASA Astrophysics Data System (ADS)

Pinto, C.; Galdámez, A.; Barahona, P.; Moris, S.; Peña, O.

2018-06-01

Selenospinels, CuCr2-xMxSe4 (M = Zr and Sn), were synthesized via conventional solid-state reactions. The crystal structure of CuCr1.5Sn0.5Se4, CuCr1.7Sn0.3Se4, CuCr1.5Zr0.5Se4, and CuCr1.8Zr0.2Se4 were determined using single-crystal X-ray diffraction. All the phases crystallized in a cubic spinel-type structure. The chemical compositions of the single-crystals were examined using energy-dispersive X-ray analysis (EDS). Powder X-ray diffraction patterns of CuCr1.3Sn0.7Se4 and CuCr1.7Sn0.3Se4 were consistent with phases belonging to the Fd 3 bar m Space group. An analysis of the vibrational properties on the single-crystals was performed using Raman scattering measurements. The magnetic properties showed a spin glass behavior with increasing Sn content and ferromagnetic order for CuCr1.7Sn0.3Se4.

Improvement of crystal identification performance for a four-layer DOI detector composed of crystals segmented by laser processing

NASA Astrophysics Data System (ADS)

Mohammadi, Akram; Inadama, Naoko; Yoshida, Eiji; Nishikido, Fumihiko; Shimizu, Keiji; Yamaya, Taiga

2017-09-01

We have developed a four-layer depth of interaction (DOI) detector with single-side photon readout, in which segmented crystals with the patterned reflector insertion are separately identified by the Anger-type calculation. Optical conditions between segmented crystals, where there is no reflector, affect crystal identification ability. Our objective of this work was to improve crystal identification performance of the four-layer DOI detector that uses crystals segmented with a recently developed laser processing technique to include laser processed boundaries (LPBs). The detector consisted of 2 × 2 × 4mm3 LYSO crystals and a 4 × 4 array multianode photomultiplier tube (PMT) with 4.5 mm anode pitch. The 2D position map of the detector was calculated by the Anger calculation method. At first, influence of optical condition on crystal identification was evaluated for a one-layer detector consisting of a 2 × 2 crystal array with three different optical conditions between the crystals: crystals stuck together using room temperature vulcanized (RTV) rubber, crystals with air coupling and segmented crystals with LPBs. The crystal array with LPBs gave the shortest distance between crystal responses in the 2D position map compared with the crystal array coupled with RTV rubber or air due to the great amount of cross-talk between segmented crystals with LPBs. These results were used to find optical conditions offering the optimum distance between crystal responses in the 2D position map for the four-layer DOI detector. Crystal identification performance for the four-layer DOI detector consisting of an 8 × 8 array of crystals segmented with LPBs was examined and it was not acceptable for the crystals in the first layer. The crystal identification was improved for the first layer by changing the optical conditions between all 2 × 2 crystal arrays of the first layer to RTV coupling. More improvement was observed by combining different optical conditions between all crystals of the first layer and some crystals of the second and the third layers of the segmented array.

Crystal structure of 4,4′-(disulfanediyl)dibutanoic acid–4,4′-bipyridine (1/1)

PubMed Central

Atria, Ana María; Garland, Maria Teresa; Baggio, Ricardo

2014-01-01

4,4′-(Disulfanediyl)dibutanoic acid (dtba) and 4,4′-bipyridine (4,4′-bpy) crystallize in an 1:1 ratio, leading to the title co-crystal with composition C8H14O4S2·C10H8N2. A distinctive feature of the crystal structure is the geometry of the dtba moiety, which appears to be stretched [with a 9.98 (1) Å span between outermost carbons] and acts as an hydrogen-bonding connector, forming linear chains along [-211] with the 4,4′-bpy moiety by way of O—H⋯N hydrogen bonds and C—H⋯O interactions. The influence of the mol­ecular shape on the hydrogen-bonding pattern is analysed by comparing the title compound and two other 4,4′-bpy co-crystals with closely related mol­ecules of similar formulation but different geometry, showing the way in which this correlates with the packing arrangement. PMID:25309167

Amplify Interest in STS.

ERIC Educational Resources Information Center

Chiappetta, Eugene L; Mays, John D.

1992-01-01

Presents activities in which students construct simple crystal radio sets and amplifiers out of diodes, transistors, and integrated circuits. Provides conceptual background, materials needed, instructions, diagrams, and classroom applications. (MDH)

Separation and Precipitation of Nickel from Acidic Sulfate Leaching Solution of Molybdenum-Nickel Black Shale by Potassium Nickel Sulfate Hexahydrate Crystallization

NASA Astrophysics Data System (ADS)

Deng, Zhigan; Wei, Chang; Fan, Gang; Li, Xingbin; Li, Minting; Li, Cunxiong

2018-02-01

Nickel was separated and precipitated with potassium nickel sulfate hexahydrate [K2Ni(SO4)2·6H2O] from acidic sulfate solution, a leach solution from molybdenum-nickel black shale. The effects of the potassium sulfate (K2SO4) concentration, crystallization temperature, solution pH, and crystallization time on nickel(II) recovery and iron(III) precipitation were investigated, revealing that nickel and iron were separated effectively. The optimum parameters were K2SO4 concentration of 200 g/L, crystallization temperature of 10°C, solution pH of 0.5, and crystallization time of 24 h. Under these conditions, 97.6% nickel(II) was recovered as K2Ni(SO4)2·6H2O crystals while only 2.0% of the total iron(III) was precipitated. After recrystallization, 98.4% pure K2Ni(SO4)2·6H2O crystals were obtained in the solids. The mother liquor was purified by hydrolysis-precipitation followed by cooling, and more than 99.0% K2SO4 could be crystallized. A process flowsheet was developed to separate iron(III) and nickel(II) from acidic-sulfate solution.

Studies on the in vitro and in vivo antiurolithic activity of Holarrhena antidysenterica

PubMed Central

Khan, Aslam; Khan, Saeed R.; Gilani, Anwar H.

2013-01-01

Background Holarrhena antidysenterica has a traditional use in the treatment of urolithiasis, therefore, its crude extract has been investigated for possible antiurolithic effect. Materials and methods The crude aqueous-methanolic extract of Holarrhena antidysenterica (Ha.Cr) was studied using the in vitro and in vivo methods. Results In the in vitro experiments, Ha.Cr demonstrated a concentration-dependent (0.25–4 mg/ml) inhibitory effect on the slope of aggregation. It decreased the size of crystals and transformed the calcium oxalate monohydrate (COM) to calcium oxalate dehydrate (COD) crystals, in calcium oxalate metastable solutions. It also showed concentration-dependent antioxidant effect against 2,2-diphenyl-1-picrylhydrazyl free radical (DPPH) free radicals and lipid peroxidation induced in rat kidney tissue homogenate. Ha.Cr (0.3 mg/ml) reduced (p < 0.05) the cell toxicity and LDH release in renal epithelial cells (MDCK) exposed to oxalate (0.5 mM) and COM (66 μg/cm2) crystals. In male Wistar rats, receiving 0.75% ethylene glycol (EG) for 21 days along with 1% ammonium chloride (AC) in drinking water, Ha.Cr treatment (30–100 mg/kg) prevented the toxic changes caused by lithogenic agents; EG and AC, like loss of body weight, polyurea, oxaluria, raised serum urea and creatinine levels and crystal deposition in kidneys compared to their respective controls. Conclusion These data indicate that Holarrhena antidysenterica possesses antiurolithic activity, possibly mediated through inhibition of CaOx crystal aggregation, antioxidant and renal epithelial cell protective activities and may provide base for designing future studies to establish its efficacy and safety for clinical use. PMID:22622371

Three's company: co-crystallization of a self-assembled S(4) metallacyclophane with two diastereomeric metallacycle intermediates.

PubMed

Lindquist, Nathan R; Carter, Timothy G; Cangelosi, Virginia M; Zakharov, Lev N; Johnson, Darren W

2010-05-28

Three discrete supramolecular self-assembled arsenic(iii) complexes including an unusual S(4)-symmetric tetranuclear [As(4)L(2)Cl(4)] metallacyclophane and two diastereomeric cis/trans-[As(2)LCl(2)] metallacycle intermediates co-crystallize within a single crystal lattice.

Synthesis and structural study of 4-(2-chlorophenyl)-2-ethoxy-5,6,7,8,9,10-hexahydrocycloocta[B] pyridine-3-carbonitrile

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

Fathima, K. Saiadali; Vasumathi, M.; Anitha, K., E-mail: singlecrystalxrd@gmail.com

2016-05-23

The novel organic material C{sub 20}H{sub 21}ClN{sub 2}O was synthesized by One-Pot synthesis method and the single crystals were grown by slow evaporation solution growth technique. The crystal structure was elucidated by subjecting the grown crystals to the single crystal x-ray diffraction analysis and was refined by full matrix least-squares method to R=0.039 for 2746 reflections. Crystal system of the grown crystal was found to be monoclinic with the space group P2{sub 1}/a and a=9.196(4) Å, b=13.449(4) Å, c=14.818(4) Å, β= 101.542(3)°, V=1795.6(11) Å{sup 3} and Z=4. In this crystal structure, cyclooctanone prefers to reside in a chair-boat conformation. Themore » structure is stabilized by attractive molecular force such as CH/π interaction called hydrophobic interaction.« less

Dipole moment and solvatochromism of benzoic acid liquid crystals: Tuning the dipole moment and molecular orbital energies by substituted Au under external electric field

NASA Astrophysics Data System (ADS)

Sıdır, Yadigar Gülseven; Sıdır, İsa; Demiray, Ferhat

2017-06-01

The optical absorption and steady-state fluorescence spectra of 4-heptyloxybenzoic acid (4hoba), 4-octyloxybenzoic acid (4ooba) and 4-nonyloxybenzoic acid (4noba) liquid crystals have been measured in a series of different polarity organic solvents. The ground state (μg) and excited state (μe) dipole moments of the monomeric and dimeric 4-alkyloxybenzoic acid liquid crystals have been obtained by means of different solvatochromic shift methods. HOMO-LUMO gaps (HLG) and dipole moments have been tuned by applying external electric (EF) field on monomer, dimer and Au substituted monomer and dimer liquid crystal structures. By applying external electric field, Au substituted monomer liquid crystals display semiconductor character, while Au substituted dimer liquid crystals gain metallic character under E = 0.04 V/Å. Eventuated specific and non-specific interactions between solvent and solute in solvent medium have been expounded by using LSER (Linear Solvation Energy Relationships).

A 2D/3D hybrid integral imaging display by using fast switchable hexagonal liquid crystal lens array

NASA Astrophysics Data System (ADS)

Lee, Hsin-Hsueh; Huang, Ping-Ju; Wu, Jui-Yi; Hsieh, Po-Yuan; Huang, Yi-Pai

2017-05-01

The paper proposes a new display which could switch 2D and 3D images on a monitor, and we call it as Hybrid Display. In 3D display technologies, the reduction of image resolution is still an important issue. The more angle information offer to the observer, the less spatial resolution would offer to image resolution because of the fixed panel resolution. Take it for example, in the integral photography system, the part of image without depth, like background, will reduce its resolution by transform from 2D to 3D image. Therefore, we proposed a method by using liquid crystal component to quickly switch the 2D image and 3D image. Meanwhile, the 2D image is set as a background to compensate the resolution.. In the experiment, hexagonal liquid crystal lens array would be used to take the place of fixed lens array. Moreover, in order to increase lens power of the hexagonal LC lens array, we applied high resistance (Hi-R) layer structure on the electrode. Hi-R layer would make the gradient electric field and affect the lens profile. Also, we use panel with 801 PPI to display the integral image in our system. Hence, the consequence of full resolution 2D background with the 3D depth object forms the Hybrid Display.

Synthesis, crystal growth and studies on non-linear optical property of new chalcones

NASA Astrophysics Data System (ADS)

Sarojini, B. K.; Narayana, B.; Ashalatha, B. V.; Indira, J.; Lobo, K. G.

2006-09-01

The synthesis, crystal growth and non-linear optical (NLO) property of new chalcone derivatives are reported. 4-Propyloxy and 4-butoxy benzaldehydes were made to under go Claisen-Schmidt condensation with 4-methoxy, 4-nitro and 4-phenoxy acetophenones to form corresponding chalcones. The newly synthesized compounds were characterized by analytical and spectral data. The Second harmonic generation (SHG) efficiency of these compounds was measured by powder technique using Nd:YAG laser. Among tested compounds three chalcones showed NLO property. The chalcone 1-(4-methoxyphenyl)-3-(4-propyloxy phenyl)-2-propen-1-one exhibited SHG conversion efficiency 2.7 times that of urea. The bulk crystal of 1-(4-methoxyphenyl)-3-(4-butoxyphenyl)-2-propen-1-one (crystal size 65×28×15 mm 3) was grown by slow-evaporation technique from acetone. Microhardness of the crystal was tested by Vicker's microhardness method.

Effect of Li and NH4 doping on the crystal perfection, second harmonic generation efficiency and laser damage threshold of potassium pentaborate crystals

NASA Astrophysics Data System (ADS)

Vigneshwaran, A. N.; Kalainathan, S.; Raja, C. Ramachandra

2018-03-01

Potassium pentaborate (KB5) is an excellent nonlinear optical material especially in the UV region. In this work, Li and NH4 doped KB5 crystals were grown using slow evaporation solution growth method. The incorporation of dopant has been confirmed and analysed by Energy dispersive X-ray analysis (EDAX), Inductively coupled plasma (ICP) analysis and Raman spectroscopy. The crystalline perfection of pure and doped KB5 crystals was studied by High resolution X-ray diffraction (HRXRD) analysis. Structural grain boundaries were observed in doped crystals. Second harmonic generation was confirmed for pure and doped crystals and output values revealed the enhancement of SHG efficiency in doped crystals. Resistance against laser damage was carried out using 1064 nm Nd-YAG laser of pulse width 10 ns. The laser damage threshold value is increased in Li doped crystal and decreased in NH4 doped crystal when compared to pure KB5 crystal.

Absolute structure and structure-function relationships of 4R,2‧R and 4S,2‧S Pidotimod®

NASA Astrophysics Data System (ADS)

Sarno, Simone; Manzo, Angelo M.; Ferraris, Davide M.; Miggiano, Riccardo; Rizzi, Menico; Palin, Luca; Boccaleri, Enrico; Milanesio, Marco

2017-11-01

Pidotimod® is a dipeptide with widely recognized immunomodulatory properties and with particularly beneficial effects for the treatment of acute respiratory and urinary tract infections. Pidotimod® presents two chiral centres which originate four stereoisomers. (4R,2‧S, 4S,2‧R, 4R,2‧R and 4S,2‧S). To date, only the 4R,2‧S and 4S,2‧R stereoisomers are reported in the literature. We report here the absolute crystal structure of the 4R,2‧R and 4S,2‧S diastereoisomers of Pidotimod®, obtained by crystals grown by slow evaporation of a mixture of water and ethanol. The analysis of the crystal structures revealed the key role of a solvent water molecule in the crystal packing engaged in an extended hydrogen bonds network. This water-assisted H-bond network explained the recalcitrance of 4R,2‧R and 4S,2‧S Pidotimod® to crystallize in pure ethanol, despite their high solubility, and the growth of well-diffracting crystals only in presence of water. Hence, Pidotimod®4R,2‧R and 4S,2‧S stereoisomers markedly differ from the 4R,2‧S and 4S,2‧R ones, which crystallize in absence of water. The molecular and crystal structures of the 4R,2‧R and 4S,2‧S Pidotimod® stereoisomers here presented gave some hints on the differences in bioactivity with respect to the 4R,2‧S stereoisomer. In fact, beyond an expected different dispositions of hydrophilic ligands, 4R,2‧R and 4S,2‧S showed an incremented tendency to intermolecular H-bonds with water.

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.

Crystallization of chicken egg white lysozyme from assorted sulfate salts

NASA Astrophysics Data System (ADS)

Forsythe, Elizabeth L.; Snell, Edward H.; Malone, Christine C.; Pusey, Marc L.

1999-01-01

Chicken egg white lysozyme has been found to crystallize from ammonium, sodium, potassium, rubidium, magnesium, and manganese sulfates at acidic and basic pH, with protein concentrations from 60 to 190 mg/ml. Crystals have also been grown at 4°C in the absence of any other added salts using isoionic lysozyme which was titrated to pH 4.6 with dilute sulfuric acid. Four different crystal forms have been obtained, depending upon the temperature, protein concentration, and precipitating salt employed. Crystals grown at 15°C were generally tetragonal, with space group P4 32 12. Crystallization at 20°C typically resulted in the formation of orthorhombic crystals, space group P2 12 12 1. The tetragonal ↔ orthorhombic transition appeared to be a function of both the temperature and protein concentration, occurring between 15 and 20°C and between 100 and 125 mg/ml protein concentration. Crystallization from 1.2 M magnesium sulfate at pH 7.8 gave a trigonal crystal, space group P3 12 1, a= b=87.4, c=73.7, γ=120°, which diffracted to 2.8 Å. Crystallization from ammonium sulfate at pH 4.6, generally at lower temperatures, was also found to result in a monoclinic form, space group C2, a=65.6, b=95.0, c=41.2, β=119.2°. A crystal of ˜0.2×0.2×0.5 mm grown from bulk solution diffracted to ˜3.5 Å.

Raster-scanning serial protein crystallography using micro- and nano-focused synchrotron beams

PubMed Central

Coquelle, Nicolas; Brewster, Aaron S.; Kapp, Ulrike; Shilova, Anastasya; Weinhausen, Britta; Burghammer, Manfred; Colletier, Jacques-Philippe

2015-01-01

High-resolution structural information was obtained from lysozyme microcrystals (20 µm in the largest dimension) using raster-scanning serial protein crystallography on micro- and nano-focused beamlines at the ESRF. Data were collected at room temperature (RT) from crystals sandwiched between two silicon nitride wafers, thereby preventing their drying, while limiting background scattering and sample consumption. In order to identify crystal hits, new multi-processing and GUI-driven Python-based pre-analysis software was developed, named NanoPeakCell, that was able to read data from a variety of crystallographic image formats. Further data processing was carried out using CrystFEL, and the resultant structures were refined to 1.7 Å resolution. The data demonstrate the feasibility of RT raster-scanning serial micro- and nano-protein crystallography at synchrotrons and validate it as an alternative approach for the collection of high-resolution structural data from micro-sized crystals. Advantages of the proposed approach are its thriftiness, its handling-free nature, the reduced amount of sample required, the adjustable hit rate, the high indexing rate and the minimization of background scattering. PMID:25945583

SABRE: Dark matter annual modulation detection in the northern and southern hemispheres

NASA Astrophysics Data System (ADS)

Tomei, C.

2017-02-01

SABRE (Sodium-iodide with Active Background REjection) is a new NaI(Tl) experiment designed to search for galactic Dark Matter through the annual modulation signature. SABRE will consist of highly pure NaI(Tl) crystals operated in an active liquid scintillator veto. The SABRE experiment will follow a two-phase approach. In the first phase, one high-purity NaI(Tl) crystal will be operated at LNGS in an active liquid scintillator veto with the goal of demonstrating backgrounds low enough for a sensitive test of the DAMA/LIBRA result. An unprecedented radio-purity for both the NaI powder and the crystal growth will be needed to achieve this goal. The second phase will consist in building two high-purity NaI(Tl) detector arrays, with a total mass of about 50 kg each, located at LNGS and in the Stawell Gold Mine in Australia. The operation of twin full-scale experiments in both the northern and the southern hemispheres will strengthen the reliability of the result against any possible seasonal systematic effect.

Raster-scanning serial protein crystallography using micro- and nano-focused synchrotron beams

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

Coquelle, Nicolas; Brewster, Aaron S.; Kapp, Ulrike

High-resolution structural information was obtained from lysozyme microcrystals (20 µm in the largest dimension) using raster-scanning serial protein crystallography on micro- and nano-focused beamlines at the ESRF. Data were collected at room temperature (RT) from crystals sandwiched between two silicon nitride wafers, thereby preventing their drying, while limiting background scattering and sample consumption. In order to identify crystal hits, new multi-processing and GUI-driven Python-based pre-analysis software was developed, named NanoPeakCell, that was able to read data from a variety of crystallographic image formats. Further data processing was carried out using CrystFEL, and the resultant structures were refined to 1.7 Åmore » resolution. The data demonstrate the feasibility of RT raster-scanning serial micro- and nano-protein crystallography at synchrotrons and validate it as an alternative approach for the collection of high-resolution structural data from micro-sized crystals. Advantages of the proposed approach are its thriftiness, its handling-free nature, the reduced amount of sample required, the adjustable hit rate, the high indexing rate and the minimization of background scattering.« less

Raster-scanning serial protein crystallography using micro- and nano-focused synchrotron beams.

PubMed

Coquelle, Nicolas; Brewster, Aaron S; Kapp, Ulrike; Shilova, Anastasya; Weinhausen, Britta; Burghammer, Manfred; Colletier, Jacques Philippe

2015-05-01

High-resolution structural information was obtained from lysozyme microcrystals (20 µm in the largest dimension) using raster-scanning serial protein crystallography on micro- and nano-focused beamlines at the ESRF. Data were collected at room temperature (RT) from crystals sandwiched between two silicon nitride wafers, thereby preventing their drying, while limiting background scattering and sample consumption. In order to identify crystal hits, new multi-processing and GUI-driven Python-based pre-analysis software was developed, named NanoPeakCell, that was able to read data from a variety of crystallographic image formats. Further data processing was carried out using CrystFEL, and the resultant structures were refined to 1.7 Å resolution. The data demonstrate the feasibility of RT raster-scanning serial micro- and nano-protein crystallography at synchrotrons and validate it as an alternative approach for the collection of high-resolution structural data from micro-sized crystals. Advantages of the proposed approach are its thriftiness, its handling-free nature, the reduced amount of sample required, the adjustable hit rate, the high indexing rate and the minimization of background scattering.

Raster-scanning serial protein crystallography using micro- and nano-focused synchrotron beams

DOE PAGES

Coquelle, Nicolas; Brewster, Aaron S.; Kapp, Ulrike; ...

2015-04-25

High-resolution structural information was obtained from lysozyme microcrystals (20 µm in the largest dimension) using raster-scanning serial protein crystallography on micro- and nano-focused beamlines at the ESRF. Data were collected at room temperature (RT) from crystals sandwiched between two silicon nitride wafers, thereby preventing their drying, while limiting background scattering and sample consumption. In order to identify crystal hits, new multi-processing and GUI-driven Python-based pre-analysis software was developed, named NanoPeakCell, that was able to read data from a variety of crystallographic image formats. Further data processing was carried out using CrystFEL, and the resultant structures were refined to 1.7 Åmore » resolution. The data demonstrate the feasibility of RT raster-scanning serial micro- and nano-protein crystallography at synchrotrons and validate it as an alternative approach for the collection of high-resolution structural data from micro-sized crystals. Advantages of the proposed approach are its thriftiness, its handling-free nature, the reduced amount of sample required, the adjustable hit rate, the high indexing rate and the minimization of background scattering.« less

Inkjet Printing Based Mono-layered Photonic Crystal Patterning for Anti-counterfeiting Structural Colors

PubMed Central

Nam, Hyunmoon; Song, Kyungjun; Ha, Dogyeong; Kim, Taesung

2016-01-01

Photonic crystal structures can be created to manipulate electromagnetic waves so that many studies have focused on designing photonic band-gaps for various applications including sensors, LEDs, lasers, and optical fibers. Here, we show that mono-layered, self-assembled photonic crystals (SAPCs) fabricated by using an inkjet printer exhibit extremely weak structural colors and multiple colorful holograms so that they can be utilized in anti-counterfeit measures. We demonstrate that SAPC patterns on a white background are covert under daylight, such that pattern detection can be avoided, but they become overt in a simple manner under strong illumination with smartphone flash light and/or on a black background, showing remarkable potential for anti-counterfeit techniques. Besides, we demonstrate that SAPCs yield different RGB histograms that depend on viewing angles and pattern densities, thus enhancing their cryptographic capabilities. Hence, the structural colorations designed by inkjet printers would not only produce optical holograms for the simple authentication of many items and products but also enable a high-secure anti-counterfeit technique. PMID:27487978

Synthesis of three new thiophene condensed pyrene derivatives, crystal structure and evaluation of their photophysical properties

NASA Astrophysics Data System (ADS)

Moriguchi, Tetsuji; Yakeya, Daisuke; Tsuge, Akihiko; Jalli, Venkataprasad

2018-04-01

Three new thiophene condensed fluorescent pyrene derivatives have been synthesized by a two-step process, via. Wittig reaction followed by iodine promoted photocyclization. These molecules have been characterized by 1H NMR and EI-MS. Further, the molecular structures of 4a, 4b and 4c has been confirmed by single crystal X-ray diffraction analysis. The protons located in the fjord and cove-regions of molecules 4b and 4c showed downfield shifts of the protons. Molecule 4a crystallized under monoclinic system with space group P21/c, molecule 4b crystallized under monoclinic system with space group C2/c and the molecule 4c crystalized under triclinic system with space group P-1. Molecules 4a, 4b and 4c showed strong absorption maxima wavelengths at 305, 358 and 330 nm, respectively. The molar extinctinction coefficients (ε) of the compounds 4a, 4b and 4c indicated molecule 4c has better ability to absorb UV light, molecule 4b has better fluorescence intensity than molecule 4a and 4c.

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

Park, HyangKyu

The AMoRE (Advanced Mo based Rare process Experiment) collaboration is going to use calcium molybdate crystals to search for neutrinoless double beta decay of {sup 100}Mo isotope. In order to make the crystal, we use calcium carbonate and molybdenum oxide powders as raw materials. Therefore it is highly necessary to reduce potential sources for radioactive backgrounds such as U and Th in the powders. In this talk, we will present our studies for purification of calcium carbonate and molybdenum oxide powders.

Further Improvement of the RITS Code for Pulsed Neutron Bragg-edge Transmission Imaging

NASA Astrophysics Data System (ADS)

Sato, H.; Watanabe, K.; Kiyokawa, K.; Kiyanagi, R.; Hara, K. Y.; Kamiyama, T.; Furusaka, M.; Shinohara, T.; Kiyanagi, Y.

The RITS code is a unique and powerful tool for a whole Bragg-edge transmission spectrum fitting analysis. However, it has had two major problems. Therefore, we have proposed methods to overcome these problems. The first issue is the difference in the crystallite size values between the diffraction and the Bragg-edge analyses. We found the reason was a different definition of the crystal structure factor. It affects the crystallite size because the crystallite size is deduced from the primary extinction effect which depends on the crystal structure factor. As a result of algorithm change, crystallite sizes obtained by RITS drastically approached to crystallite sizes obtained by Rietveld analyses of diffraction data; from 155% to 110%. The second issue is correction of the effect of background neutrons scattered from a specimen. Through neutron transport simulation studies, we found that the background components consist of forward Bragg scattering, double backward Bragg scattering, and thermal diffuse scattering. RITS with the background correction function which was developed through the simulation studies could well reconstruct various simulated and experimental transmission spectra, but refined crystalline microstructural parameters were often distorted. Finally, it was recommended to reduce the background by improving experimental conditions.

Growth and spectroscopic properties of Tm3+:NaBi(MoO4)2 single crystal

NASA Astrophysics Data System (ADS)

Gusakova, N. V.; Mudryi, A. V.; Demesh, M. P.; Yasukevich, A. S.; Pavlyuk, A. A.; Kornienko, A. A.; Dunina, E. B.; Khodasevich, I. A.; Orlovich, V. A.; Kuleshov, N. V.

2018-06-01

In this work we report the spectroscopic properties of Tm3+:NaBi(MoO4)2 crystals with the dopant concentrations of 0.7 at.% and 3 at.%. The energy levels of the Tm3+ in the NaBi(MoO4)2 host were determined from polarized optical absorption and photoluminescence spectra measured at 77.4 K. Radiative properties of the crystals were calculated in context of Judd-Ofelt theory. Raman spectra of the crystal were studied. The concentration dependences of emission decay times of 3H4 and 3F4 levels were analyzed. The potential of the crystal for building tunable and ultrafast pulse lasers is shown on the base of cross sections and gain coefficient in the range of 1.9 μm.

Resonance electronic Raman scattering in rare earth crystals

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

Williams, G.M.

1988-11-10

The intensities of Raman scattering transitions between electronic energy levels of trivalent rare earth ions doped into transparent crystals were measured and compared to theory. A particle emphasis was placed on the examination of the effect of intermediate state resonances on the Raman scattering intensities. Two specific systems were studied: Ce/sup 3 +/(4f/sup 1/) in single crystals of LuPO/sub 4/ and Er/sup 3 +/(4f/sup 11/) in single crystals of ErPO/sub 4/. 134 refs., 92 figs., 33 tabs.

Aqueous Sulfate Separation by Sequestration of [(SO 4) 2(H 2O) 4] 4 Clusters within Highly Insoluble Imine-Linked Bis-Guanidinium Crystals

DOE PAGES

Custelcean, Radu; Williams, Neil J.; Seipp, Charles A.; ...

2015-12-18

Quantitative removal of sulfate from seawater was achieved by selective crystallization of the anion with a bis(guanidinium) ligand self-assembled in situ through imine condensation of simple components. The resulting crystalline salt has an exceptionally low aqueous solubility, on a par with BaSO 4. Single-crystal X-ray diffraction analysis revealed pairs of sulfate anions clustered together with four water molecules within the crystals.

An evaluation of adhesive sample holders for advanced crystallographic experiments

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

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

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

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.

Non-radiation induced signals in TL dosimetry.

PubMed

German, U; Weinstein, M

2002-01-01

One source of background signals, which are non-radiation related, is the reader system and it includes dark current, external contaminants and electronic spikes. These factors can induce signals equivalent to several hundredths of mSv. Mostly, the effects are minimised by proper design of the TLD reader, but some effects are dependent on proper operation of the system. The other main group of background signals originates in the TL crystal and is due to tribothermoluminescence, dirt, chemical reactions and stimulation by visible or UV light. These factors can have a significant contribution, equivalent to over several mSv, depending on whether the crystal is bare or protected by PTFE. Working in clean environments, monitoring continuously the glow curves and performing glow curve deconvolution are suggested to minimise non-radiation induced spurious signals.

Concomitant and conformational polymorphism in 4‧-(isoquinolyl-2,2‧:6‧,2″-terpyridine and 4‧-(4-quinolyl)-2,2‧:6‧,2″-terpyridine

NASA Astrophysics Data System (ADS)

Njogu, Eric M.; Nyamori, Vincent O.; Omondi, Bernard

2018-02-01

The occurrence of concomitant polymorphism in 4‧-(isoquinolyl)-2,2‧:6‧,2″-terpyridine, 1a and 1b (2-quinterpy) and conformational polymorphism in 4‧-(4-quinolyl)-2,2‧:6‧,2″-terpyridine (4-quinterpy) has been identified to due to crystallization process and solvent, respectively. Crystallization of 2-quinterpy in acetone yielded the concomitant polymorphs 1a and 1b which crystallize in the monoclinic P21/c and the orthorhombic Pna21 space groups, respectively. The polymorph 2a was grown from bulk 4-quinterpy in dimethyl sulfoxide, crystallizes in the monoclinic P21/c space group, while 2b grown from acetonitrile or even acetone crystallizes in the monoclinic system but in P21/n space group.

High resolution time-to-space conversion of sub-picosecond pulses at 1.55µm by non-degenerate SFG in PPLN crystal.

PubMed

Shayovitz, Dror; Herrmann, Harald; Sohler, Wolfgang; Ricken, Raimund; Silberhorn, Christine; Marom, Dan M

2012-11-19

We demonstrate high resolution and increased efficiency background-free time-to-space conversion using spectrally resolved non-degenerate and collinear SFG in a bulk PPLN crystal. A serial-to-parallel resolution factor of 95 and a time window of 42 ps were achieved. A 60-fold increase in conversion efficiency slope compared with our previous work using a BBO crystal [D. Shayovitz and D. M. Marom, Opt. Lett. 36, 1957 (2011)] was recorded. Finally the measured 40 GHz narrow linewidth of the output SFG signal implies the possibility to extract phase information by employing coherent detection techniques.

SABRE - A test of DAMA with high-purity NaI(Tl) crystals

NASA Astrophysics Data System (ADS)

Xu, Jingke; Calaprice, Frank; Froborg, Francis; Shields, Emily; Suerfu, Burkhant

2015-08-01

The dark matter claim by DAMA is both significant and controversial. Several experiments have claimed to rule out DAMA/LIBRA, but the comparisons are made based on dark matter halo and dark matter-interaction models that are currently unknown. Therefore, an unambiguous test of DAMA/LIBRA is best made using NaI(Tl) crystals with lower residual background than that of DAMA/LIBRA, and the SABRE experiment is designed to achieve this goal. In this paper we will discuss the development of high-purity SABRE NaI(Tl) crystals and detectors, and progress of the SABRE experiment toward testing DAMA/LIBRA.

Crystallization and photoluminescence properties of α-RE2(WO4)3 (RE: Gd, Eu) in rare-earth tungsten borate glasses

NASA Astrophysics Data System (ADS)

Wang, Yong; Honma, Tsuyoshi; Komatsu, Takayuki

2013-03-01

Glasses with the compositions of 22.5RE2O3-47.5WO3-30B2O3 (mol%) (RE: Gd, Eu) were prepared by a conventional melt quenching method, and α-Gd2(WO4)3 and α-Eu2(WO4)3 crystals were synthesized through their crystallization. The two types of WO4 tetrahedra present in α-RE2(WO4)3 provide the Raman bands at 931-934 cm-1 for WIIO4 tetrahrdra with much distortions and at 946-950 cm-1 for WIO4 tetrahedra with a near regular symmetry. The crystallized samples containing α-Eu2(WO4)3 exhibit strong red emissions under the excitation at 396 and 467 nm, although the base glass has no photoluminescence emission. α-Gd2(WO4)3 and α-Eu2(WO4)3 crystals were patterned on the glass surface by irradiations of a continuous wave Yb:YVO4 fiber laser (wavelength: 1080 nm).

Quasiperiodic Strain Bursts and Self-Organization in Crystal Microplasticity (PREPRINT)

DTIC Science & Technology

2012-03-01

AFRL-RX-WP-TP-2012-0249 QUASIPERIODIC STRAIN BURSTS AND SELF- ORGANIZATION IN CRYSTAL MICROPLASTICITY (PREPRINT) D.M. Dimiduk Metals...2012 4. TITLE AND SUBTITLE QUASIPERIODIC STRAIN BURSTS AND SELF-ORGANIZATION IN CRYSTAL MICROPLASTICITY (PREPRINT) 5a. CONTRACT NUMBER In-house...18 Quasiperiodic strain bursts and self-organization in crystal microplasticity S. Papanikolaou,1,2∗ D. M. Dimiduk,3 W. Choi4, J. P. Sethna4, M. D

Effects of the background electrolyte on Th(IV) sorption to muscovite mica

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

Schmidt, Moritz; Hellebrandt, Stefan; Knope, Karah E.

2015-09-01

The adsorption of tetravalent thorium on the muscovite mica (001) basal plane was studied by X-ray crystal truncation rod (CTR), and resonant anomalous X-ray reflectivity (RAXR) measurements and alpha spectrometry in the presence of perchlorate background electrolytes LiClO 4, NaClO 4, and KClO 4 ([Th(IV)] = 0.1 mM, I = 0.1 M or 0.01 M, pH = 3.3 ± 0.3). RAXR data directly reveal a strong influence of the background electrolyte on the actinide sorption. No significant Th adsorption was observed in 0.1 M NaClO 4, i.e., the Th coverage θ(Th), the number of Th per unit cell area ofmore » the muscovite surface (A UC = 46.72 Å 2), was ≤ 0.01 Th/A UC, whereas limited uptake (θ(Th) ~ 0.04 Th/A UC) was detected at a lower ionic strength (I = 0.01 M). These results are in stark contrast to the behavior of Th in 0.1 M NaCl which showed a coverage of 0.4 Th/A UC (Schmidt et al., 2012a). Th uptake was also influenced by the electrolyte cation. Weak adsorption was observed in 0.1M KClO 4 (θ(Th) ~ 0.07 Th/AUC) similar to the results in NaClO 4 at lower ionic strength. In contrast, strong adsorption was found in 0.1 M LiClO 4, with θ(Th) = 4.9 Th/A UC, a ~10-fold increase compared with that previously reported in NaCl. These differences are confirmed independently by ex situ alpha spectrometry, which shows no measurable Th coverage in 0.1 M NaClO 4 background in contrast to a large coverage of 1.6 Th/A UC in 0.1 M LiClO 4. The CTR/RAXR analyses of Th-LiClO 4 show the sorption structure consisting of Th species that are broadly distributed, centered at heights of 4.1 Å and 29 Å distance from the interface. Neither the very large distribution height of the second species nor the high coverage can be explained with (hydrated) ionic adsorption, suggesting that the enhanced uptake is presumably due to the formation and sorption of Th nanoparticles.« less

Modeling phosphorus removal and recovery from anaerobic digester supernatant through struvite crystallization in a fluidized bed reactor.

PubMed

Rahaman, Md Saifur; Mavinic, Donald S; Meikleham, Alexandra; Ellis, Naoko

2014-03-15

The cost associated with the disposal of phosphate-rich sludge, the stringent regulations to limit phosphate discharge into aquatic environments, and resource shortages resulting from limited phosphorus rock reserves, have diverted attention to phosphorus recovery in the form of struvite (MAP: MgNH4PO4·6H2O) crystals, which can essentially be used as a slow release fertilizer. Fluidized-bed crystallization is one of the most efficient unit processes used in struvite crystallization from wastewater. In this study, a comprehensive mathematical model, incorporating solution thermodynamics, struvite precipitation kinetics and reactor hydrodynamics, was developed to illustrate phosphorus depletion through struvite crystal growth in a continuous, fluidized-bed crystallizer. A thermodynamic equilibrium model for struvite precipitation was linked to the fluidized-bed reactor model. While the equilibrium model provided information on supersaturation generation, the reactor model captured the dynamic behavior of the crystal growth processes, as well as the effect of the reactor hydrodynamics on the overall process performance. The model was then used for performance evaluation of the reactor, in terms of removal efficiencies of struvite constituent species (Mg, NH4 and PO4), and the average product crystal sizes. The model also determined the variation of species concentration of struvite within the crystal bed height. The species concentrations at two extreme ends (inlet and outlet) were used to evaluate the reactor performance. The model predictions provided a reasonably good fit with the experimental results for PO4-P, NH4-N and Mg removals. Predicated average crystal sizes also matched fairly well with the experimental observations. Therefore, this model can be used as a tool for performance evaluation and process optimization of struvite crystallization in a fluidized-bed reactor. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

Non-proportionality study of CaMoO4 and GAGG:Ce scintillation crystals using Compton coincidence technique.

PubMed

Kaewkhao, J; Limkitjaroenporn, P; Chaiphaksa, W; Kim, H J

2016-09-01

In this study, the CCT technique and nuclear instrument module (NIM) setup for the measurements of coincidence electron energy spectra of calcium molybdate (CaMoO4) and cerium doped gadolinium aluminium gallium garnet (Gd3Al2Ga3O12:Ce or GAGG:Ce) scintillation crystals were carried out. The (137)Cs irradiated gamma rays with an energy (Eγ) of 662keV was used as a radioactive source. The coincidence electron energy spectra were recorded at seven scattering angles of 30°-120°. It was found that seven corresponding electron energies were in the range of 100.5-435.4keV. The results show that, for all electron energies, the electron energy peaks of CaMoO4 crystal yielded higher number of counts than those of GAGG:Ce crystal. The electron energy resolution, the light yield and non-proportionality were also determined. It was found that the energy resolutions are inverse proportional to the square root of electron energy for both crystals. Furthermore, the results show that the light yield of GAGG:Ce crystal is much higher than that of CaMoO4 crystal. It was also found that both CaMoO4 and GAGG:Ce crystals demonstrated good proportional property in the electron energy range of 260-435.4keV. Copyright © 2016 Elsevier Ltd. All rights reserved.

Simulated characteristics of the DEGAS γ-detector array

NASA Astrophysics Data System (ADS)

Li, G. S.; Lizarazo, C.; Gerl, J.; Kojouharov, I.; Schaffner, H.; Górska, M.; Pietralla, N.; Saha, S.; Liu, M. L.; Wang, J. G.

2018-05-01

The performance of the novel HPGe-Cluster array DEGAS to be used at FAIR has been studied through GEANT4 simulations using accurate geometries of most of the detector components. The simulation framework has been tested by comparing experimental data of various detector setups. The study showed that the DEGAS system could provide a clear improvement of the photo-peak efficiency compared to the previous RISING array. In addition, the active BGO Back-catcher could greatly enhance the background suppression capability. The add-back analysis revealed that even at a γ multiplicity of six the sensitivity is improved by adding back the energy depositions of the neighboring Ge crystals.

Glass formation and crystallization in high-temperature glass-ceramics and Si3N4

NASA Technical Reports Server (NTRS)

Drummond, Charles H., III

1991-01-01

The softening of glassy grain boundaries in ceramic matrix composites and Si3N4 at high temperatures reduces mechanical strength and the upper-use temperature. By crystallizing this glass to a more refractory crystalline phase, a material which performs at higher temperatures may result. Three systems were examined: a cordierite composition with ZrO2 as a nucleating agent; celsian compositions; and yttrium silicate glasses both in bulk and intergranular in Si3N4. For the cordierite compositions, a series of metastable phases was obtained. The crystallization of these compositions was summarized in terms of metastable ternary isothermal sections. Zircon formed at the expense of ZrO2 and spinel. In SiC composites, the transformations were slower. In celsian, two polymorphs were crystallized. One phase, hexacelsian, which always crystallized, even when metastable, had an undesirable volume change. The other phase, celsian, was very difficult to crystallize. In yttrium silicate bulk glasses, similar in composition to the intergranular glass in Si3N4, a number of polymorphs of Y2Si2O7 were crystallized. The conditions under which these polymorphs formed are compared with crystallization in Si3N4.

Crystal-Physical Model of Ion Transport in Nonlinear Optical Crystals of KTiOPO4

NASA Astrophysics Data System (ADS)

Sorokin, N. I.; Shaldin, Yu. V.

2018-04-01

The ionic conductivity along the principal axes a, b, and c of the unit cell of the nonlinear-optical high-resistance KTiOPO4 single crystals (rhombic syngony, space group Pna21), which are as-grown and after thermal annealing in vacuum, has been investigated by the method of impedance spectroscopy. The crystals were grown from a solution-melt by the Czochralski method. The as-grown KTiOPO4 crystals possess a quasi-one-dimensional conductivity along the crystallographic c axis, which is caused by the migration of K+ cations: σ║ c = 1.0 × 10-5 S/cm at 573 K. Wherein the characteristics of the anisotropy of ionic conductivity of the crystals is equal to σ║ c /σ║ a = 3 and σ║ c /σ║ b = 24. The thermal annealing at 1000 K for 10 h in vacuum increases the magnitude of σ║ c of KTiOPO4 by a factor of 28 and leads to an increase in the ratio σ║ c /σ║ b = 2.1 × 103 at 573 K. A crystal-physical model of ionic transport in KTiOPO4 crystals has been proposed.

A novel fabrication of Cu{sub 2}O@Cu{sub 7}S{sub 4} core-shell micro/nanocrystals from Cu{sub 2}O temples and enhanced photocatalytic activities

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

Li, Junqi, E-mail: sfmlab@163.com; Sun, Long; Yan, Ying

2016-08-15

Highlights: • The Cu{sub 2}O@Cu{sub 7}S{sub 4} core-shell crystals maintained the same morphology with template. • The crystals exhibit enhanced photocatalytic activity than the pure Cu{sub 2}O crystals. • The photocatalytic activity of different R crystals is diverse from each other. • A possible formation mechanism has been proposed. - Abstract: Uniform and monodispersed Cu{sub 2}O@Cu{sub 7}S{sub 4} core-shell micro/nanocrystals have been synthesized successfully at room temperature via a simple chemical etching reaction, using Cu{sub 2}O as sacrificial template. The structure and properties of the crystals were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM),more » X-ray photoelectron spectra (XPS). The photocatalytic activity of the Cu{sub 2}O@Cu{sub 7}S{sub 4} crystals was evaluated by photocatalytic decolorization of MeO (methyl orange) aqueous solution at ambient temperature under visible-light irradiation. The results show that the as-prepared Cu{sub 2}O@Cu{sub 7}S{sub 4} crystals revealed core-shell structure, which maintained the same morphology with corresponding template and were composed of cuboctahedron Cu{sub 7}S{sub 4} shell and active Cu{sub 2}O core. Due to the unique Cu{sub 2}O@Cu{sub 7}S{sub 4} core-shell structure, the crystals exhibit enhanced photocatalytic activity than that of the pure Cu{sub 2}O crystals, and the photocatalytic activity of different R crystals is diverse from each other. A possible formation mechanism has been proposed.« less

Electrical conduction studies in ferric-doped KHSO 4 single crystals

NASA Astrophysics Data System (ADS)

Sharon, M.; Kalia, A. K.

1980-03-01

Direct-current conductivity of ferric-doped (138, 267, and 490 ppm) single crystals of KHSO 4 has been studied. The mechanism for the dc conduction process is discussed. It is observed that the ferric ion forms a (Fe 3+-two vacancies) complex and the enthaply for its formation is 0.09 ± 0.01 eV. It is proposed that each ferric ion removes two protons from each HSO 4 dimer. The conductivity plot shows the presence of intrinsic and extrinsic regions. It is proposed that in the intrinsic region the dimer of HSO -4 breaks reversibly to form a long-chain monomer-type structure. The conductivity in the KHSO 4 crystal is proposed to be controlled by the rotation of HSO -4 tetrahedra along the axis which contains no hydrogen atom. Isotherm calculation for the trivalent-doped system is applied to this crystal and the results are compared with Co 2+-doped KHSO 4 crystal. The distribution coefficient of ferric ion in the KHSO 4 single crystal is calculated to be 4.5 × 10 -1. Ferric ion causes tapering in the crystal growth habit of KHSO 4 and it is believed to be due to the presence of (Fe 3+-two vacancies) complex. The enthalpy values for the various other processes are as follows: enthalpy for the breakage of HSO -4 dimer ( Hi) = 1.28 ± 0.01 eV; enthalpy for the rotation of HSO -4 tetrahedron ( Hm) = 0.58 ± 0.01 eV.

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

Sundaramurthi, Prakash; Suryanarayanan, Raj

To effectively inhibit succinate buffer crystallization and the consequent pH changes in frozen solutions. Using differential scanning calorimetry (DSC) and X-ray diffractometry (XRD), the crystallization behavior of succinate buffer in the presence of either (i) a crystallizing (glycine, mannitol, trehalose) or (ii) a non-crystallizing cosolute (sucrose) was evaluated. Aqueous succinate buffer solutions, 50 or 200 mM, at pH values 4.0 or 6.0 were cooled from room temperature to -25 C at 0.5 C/min. The pH of the solution was measured as a function of temperature using a probe designed to function at low temperatures. The final lyophiles prepared from thesemore » solutions were characterized using synchrotron radiation. When the succinic acid solution buffered to pH 4.0, in the absence of a cosolute, was cooled, there was a pronounced shift in the freeze-concentrate pH. Glycine and mannitol, which have a tendency to crystallize in frozen solutions, remained amorphous when the initial pH was 6.0. Under this condition, they also inhibited buffer crystallization and prevented pH change. At pH 4.0 (50 mM initial concentration), glycine and mannitol crystallized and did not prevent pH change in frozen solutions. While sucrose, a non-crystallizing cosolute, did not completely prevent buffer crystallization, the extent of crystallization was reduced. Sucrose decomposition, based on XRD peaks attributable to {beta}-D-glucose, was observed in frozen buffer solutions with an initial pH of 4.0. Trehalose completely inhibited crystallization of the buffer components when the initial pH was 6.0 but not at pH 4.0. At the lower pH, the crystallization of both trehalose dihydrate and buffer components was evident. When retained amorphous, sucrose and trehalose effectively inhibited succinate buffer component crystallization and the consequent pH shift. However, when trehalose crystallized or sucrose degraded to yield a crystalline decomposition product, crystallization of buffer was observed. Similarly, glycine and mannitol, two widely used bulking agents, inhibited buffer component crystallization only when retained amorphous. In addition to stabilizing the active pharmaceutical ingredient, lyoprotectants may prevent solution pH shift by inhibiting buffer crystallization.« less

Growth and characterization of organic material 4-dimethylaminobenzaldehyde single crystal.

PubMed

Jebin, R P; Suthan, T; Rajesh, N P; Vinitha, G; Madhusoodhanan, U

2015-01-25

The organic material 4-dimethylaminobenzaldehyde single crystals were grown by slow evaporation technique. The grown crystal was confirmed by the single crystal and powder X-ray diffraction analyses. The functional groups of the crystal have been identified from the Fourier Transform Infrared (FTIR) and FT-Raman studies. The optical property of the grown crystal was analyzed by UV-Vis-NIR and photoluminescence (PL) spectral measurements. The thermal behavior of the grown crystal was analyzed by thermogravimetric (TG) and differential thermal analyses (DTA). Dielectric measurements were carried out with different frequencies by using parallel plate capacitor method. The third order nonlinear optical properties of 4-dimethylaminobenzaldehyde was measured by the Z-scan technique using 532 nm diode pumped continuous wave (CW) Nd:YAG laser. Copyright © 2014 Elsevier B.V. All rights reserved.

Self-powdering and nonlinear optical domain structures in ferroelastic beta'-Gd{sub 2}(MoO{sub 4}){sub 3} crystals formed in glass

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

Tsukada, Y.; Honma, T.; Komatsu, T., E-mail: komatsu@mst.nagaokaut.ac.j

Ferroelastic beta'-Gd{sub 2}(MoO{sub 4}){sub 3}, (GMO), crystals are formed through the crystallization of 21.25Gd{sub 2}O{sub 3}-63.75MoO{sub 3}-15B{sub 2}O{sub 3} glass (mol%), and two scientific curious phenomena are observed. (1) GMO crystals formed in the crystallization break into small pieces with a triangular prism or pyramid shape having a length of 50-500 {mu}m spontaneously during the crystallizations in the inside of an electric furnace, not during the cooling in air after the crystallization. This phenomenon is called 'self-powdering phenomenon during crystallization' in this paper. (2) Each self-powdered GMO crystal grain shows a periodic domain structure with different refractive indices, and amore » spatially periodic second harmonic generation (SHG) depending on the domain structure is observed. It is proposed from polarized micro-Raman scattering spectra and the azimuthal dependence of second harmonic intensities that GMO crystals are oriented in each crystal grain and the orientation of (MoO{sub 4}){sup 2-} tetrahedra in GMO crystals changes periodically due to spontaneous strains in ferroelastic GMO crystals. - Graphical abstract: This figure shows the polarized optical photograph at room temperature for a particle (piece) obtained by a heat treatment of the glass at 590 deg. C for 2 h in an electric furnace in air. This particle was obtained through the self-powdering behavior in the crystallization of glass. The periodic domain structure is observed. Ferroelastic beta'-Gd{sub 2}(MoO{sub 4}){sub 3} crystals are formed in the particle, and second harmonic generations are detected, depending on the domain structure.« less

High energy resolution, high angular acceptance crystal monochromator

DOEpatents

Alp, E.E.; Mooney, T.M.; Toellner, T.

1996-06-04

A 4-bounce dispersive crystal monochromator reduces the bandpass of synchrotron radiation to a 10-50 meV range without sacrificing angular acceptance. The monochromator includes the combination of an asymmetrical channel-cut single crystal of lower order reflection and a symmetrical channel-cut single crystal of higher order reflection in a nested geometric configuration. In the disclosed embodiment, a highly asymmetrically cut ({alpha}=20) outer silicon crystal (4 2 2) with low order reflection is combined with a symmetrically cut inner silicon crystal (10 6 4) with high order reflection to condition a hard x-ray component (5--30 keV) of synchrotron radiation down to the {micro}eV-neV level. Each of the crystals is coupled to the combination of a positioning inchworm and angle encoder via a respective rotation stage for accurate relative positioning of the crystals and precise energy tuning of the monochromator. 7 figs.

High energy resolution, high angular acceptance crystal monochromator

DOEpatents

Alp, Ercan E.; Mooney, Timothy M.; Toellner, Thomas

1996-06-04

A 4-bounce dispersive crystal monochromator reduces the bandpass of synchrotron radiation to a 10-50 meV range without sacrificing angular acceptance. The monochromator includes the combination of an asymmetrical channel-cut single crystal of lower order reflection and a symmetrical channel-cut single crystal of higher order reflection in a nested geometric configuration. In the disclosed embodiment, a highly asymmetrically cut (.alpha.=20) outer silicon crystal (4 2 2) with low order reflection is combined with a symmetrically cut inner silicon crystal (10 6 4) with high order reflection to condition a hard x-ray component (5-30 keV) of synchrotron radiation down to the .mu.eV-neV level. Each of the crystals is coupled to the combination of a positioning inchworm and angle encoder via a respective rotation stage for accurate relative positioning of the crystals and precise energy tuning of the monochromator.

The Fundamentals of Dislocation Transport of Hydrogen in BCC Iron.

DTIC Science & Technology

1984-10-01

4.2.1. Single Crystal Material 24 4.2.2. Polycrystalline Material 25 4.3. Single Crystal Orientation Determination 25 4.4. Straining Permeation Test 27...Test 45 4.6. Supersaturation Study 47 S. RESULTS AND DISCUSSION 50 5.1. Single Crystal Orientation Determination 50 5.1.1. Slip System Determination 58...Orientation 162 Determination B.1. Dislocation Line Direction Determination 162 B.2. Burgers Vector Determination 164

Growth and characterization of a third order nonlinear optical single crystal: Ethylenediamine-4-nitrophenolate monohydrate

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

Dhanalakshmi, B.; Ponnusamy, S., E-mail: suruponnus@gmail.com; Muthamizhchelvan, C.

2015-10-15

Highlights: • EDA4NPH crystal possesses negative nonlinear refractive index. • The crystal exhibits high third-order NLO susceptibility. • Wide transparency of the crystal makes it suitable for NLO applications. • Dielectric studies substantiate the suitability for electro-optic applications. • The crystal possesses suitable mechanical strength for device fabrication. - Abstract: Bulk crystals of the charge-transfer complex, ethylenediamine-4-nitrophenolate monohydrate, were grown by slow solvent evaporation method from aqueous solution at room temperature. The X-ray diffraction measurements showed that the crystal belongs to centrosymmetric space group C2/c of monoclinic system. The functional groups in the complex were identified using FTIR, FTRaman andmore » FTNMR analyses. The Z-scan measurements revealed the negative nonlinear refractive index of the crystal. The nonlinear absorption coefficient and third order nonlinear optical susceptibility calculated from the measurements were −3.5823 × 10{sup −3} cm/W and 2.3762 × 10{sup −6} esu respectively. The crystal was shown to be highly transparent above 366 nm by UV–vis spectroscopy and a yellow fluorescence was observed from PL spectrum. The TG–DTA and DSC analyses showed that the crystal is thermally stable up to 117.4 °C. The crystals were characterized by dielectric, etching and microhardness studies.« less

Localisation of gamma-ray interaction points in thick monolithic CeBr3 and LaBr3:Ce scintillators

NASA Astrophysics Data System (ADS)

Ulyanov, Alexei; Morris, Oran; Roberts, Oliver J.; Tobin, Isaac; Hanlon, Lorraine; McBreen, Sheila; Murphy, David; Nelms, Nick; Shortt, Brian

2017-02-01

Localisation of gamma-ray interaction points in monolithic scintillator crystals can simplify the design and improve the performance of a future Compton telescope for gamma-ray astronomy. In this paper we compare the position resolution of three monolithic scintillators: a 28×28×20 mm3 (length×breadth × thickness) LaBr3:Ce crystal, a 25×25×20 mm3 CeBr3 crystal and a 25×25×10 mm3 CeBr3 crystal. Each crystal was encapsulated and coupled to an array of 4×4 silicon photomultipliers through an optical window. The measurements were conducted using 81 keV and 356 keV gamma-rays from a collimated 133Ba source. The 3D position reconstruction of interaction points was performed using artificial neural networks trained with experimental data. Although the position resolution was significantly better for the thinner crystal, the 20 mm thick CeBr3 crystal showed an acceptable resolution of about 5.4 mm FWHM for the x and y coordinates, and 7.8 mm FWHM for the z-coordinate (crystal depth) at 356 keV. These values were obtained from the full position scans of the crystal sides. The position resolution of the LaBr3:Ce crystal was found to be considerably worse, presumably due to the highly diffusive optical interface between the crystal and the optical window of the enclosure. The energy resolution (FWHM) measured for 662 keV gamma-rays was 4.0% for LaBr3:Ce and 5.5% for CeBr3. The same crystals equipped with a PMT (Hamamatsu R6322-100) gave an energy resolution of 3.0% and 4.7%, respectively.

Crystal growth, structural, optical, thermal, mechanical, laser damage threshold and electrical properties of triphenylphosphine oxide 4-nitrophenol (TP4N) single crystals for nonlinear optical applications

NASA Astrophysics Data System (ADS)

Karuppasamy, P.; Senthil Pandian, Muthu; Ramasamy, P.; Verma, Sunil

2018-05-01

The optically good quality single crystals of triphenylphosphine oxide 4-nitrophenol (TP4N) with maximum dimension of 15 × 10 × 5 mm3 were grown by slow evaporation solution technique (SEST) at room temperature. The cell dimensions of the grown TP4N crystal were confirmed by single crystal X-ray diffraction (SXRD) and the crystalline purity was confirmed and planes were indexed by powder X-ray diffraction (PXRD) analysis. Functional groups of TP4N crystal were confirmed by Fourier transform infrared (FTIR) spectral analysis. The optical transmittance of the grown crystal was determined by the UV-Vis NIR spectral analysis and it has good optical transparency in the entire visible region. The band tail (Urbach) energy of the grown crystal was analyzed and it appears to be minimum, which indicates that the TP4N has good crystallinity. The position of valence band (Ev) and conduction band (Ec) of the TP4N have been determined from the electron affinity energy (EA) and the ionization energy (EI) of its elements and using the optical band gap. The thermal behaviour of the grown crystal was investigated by thermogravimetric and differential thermal analysis (TG-DTA). Vickers microhardness analysis was carried out to identify the mechanical stability of the grown crystal and their indentation size effect (ISE) was explained by the Meyer's law (ML), Hays-Kendall's (HK) approach, proportional specimen resistance (PSR) model, modified PSR model (MPSR), elastic/plastic deformation (EPD) model and indentation induced cracking (IIC) model. Chemical etching study was carried out to find the etch pit density (EPD) of the grown crystal. Laser damage threshold (LDT) value was measured by using Nd:YAG laser (1064 nm). The dielectric permittivity (ε՛) and dielectric loss (tan δ) as a function of frequency was measured. The electronic polarizability (α) of the TP4N crystal was calculated. It is well matched to the value which was calculated from Clausius-Mossotti relation, Lorentz-Lorentz equation, optical band gap and coupled dipole method (CDM). The Z-scan technique was carried out using solid state laser (640 nm) to analyze the nonlinear optical properties of the TP4N crystal. It exhibits the self-defocusing and saturable absorbance effect during analysis of closed and open aperture respectively. The nonlinear optical parameters such as refractive index (n2), absorption coefficient (β) and the third order nonlinear optical susceptibility (χ(3)) were analyzed.

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

NASA Astrophysics Data System (ADS)

Sadhasivam, S.; Rajesh, N. P.

2017-12-01

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

Crystallization of Chicken Egg White Lysozyme from Assorted Sulfate Salts

NASA Technical Reports Server (NTRS)

Forsythe, Elizabeth L.; Snell, Edward H.; Malone, Christine C.; Pusey, Marc L.

1999-01-01

Chicken egg white lysozyme has been found to crystallize from ammonium, sodium, potassium, rubidium, magnesium, and manganese sulfates at acidic and basic pH, with protein concentrations from 60 to 190 mg/ml. Crystals have also been grown at 4 C in the absence of any other added salts using isoionic lysozyme which was titrated to pH 4.6 with dilute sulfuric acid. Four different crystal forms have been obtained, depending upon the temperature, protein concentration, and precipitating salt employed. Crystals grown at 15 C were generally tetragonal, with space group P4(sub 3)2(sub 1)2. Crystallization at 20 C typically resulted in the formation of orthorhombic crystals, space group P2(sub 1)2(sub 1)2(sub 1). The tetragonal reversible reaction orthorhombic transition appeared to be a function of both the temperature and protein concentration, occurring between 15 and 20 C and between 100 and 125 mg/ml protein concentration. Crystallization from 1.2 M magnesium sulfate at pH 7.8 gave a trigonal crystal, space group P3(sub 1)2(sub 1), a = b = 87.4, c = 73.7, gamma = 120 deg, which diffracted to 2.8 A. Crystallization from ammonium sulfate at pH 4.6, generally at lower temperatures, was also found to result in a monoclinic form. space group C2, a = 65.6, b = 95.0, c = 41.2, beta = 119.2 deg. A crystal of approximately 0.2 x 0.2 x 0.5 mm grown from bulk solution diffracted to approximately 3.5 A.

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

PubMed

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

2013-07-01

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

Acousto-optic interaction in alpha-BaB(2)O(4)and Li(2)B(4)O(7) crystals.

PubMed

Martynyuk-Lototska, Irina; Mys, Oksana; Dudok, Taras; Adamiv, Volodymyr; Smirnov, Yevgen; Vlokh, Rostyslav

2008-07-01

Experimental studies and analysis of acousto-optic diffraction in alpha-BaB(2)O(4) and Li(2)B(4)O(7) crystals are given. Ultrasonic wave velocity, elastic compliance and stiffness coefficients, and piezo-optic and photoelastic coefficients of alpha-BaB(2)O(4) and Li(2)B(4)O(7) crystals are determined. The acousto-optic figure of merit has been estimated for different possible geometries of acousto-optic interaction. It is shown that the acousto-optic figures of merit for alpha-BaB(2)O(4) crystals reach the value M(2)=(270 +/- 70) x 10(-15) s(3)/kg for the case of interaction with the slowest ultrasonic wave. The directions of propagation and polarization of those acoustic waves are obtained on the basis of construction of acoustic slowness surfaces. The acousto-optic diffraction is experimentally studied for alpha-BaB(2)O(4) and Li(2)B(4)O(7) crystals.

Crystallization and initial X-ray analysis of polyhydroxyalkanoate granule-associated protein from Aeromonas hydrophila

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

Zhao, Minglian; Li, Zhenguo; Zheng, Wei

The phasin PhaP{sub Ah} from A. hydrophila strain 4AK4 was crystallized using the hanging-drop vapour-diffusion method. Polyhydroxyalkanoate (PHA) granule-associated proteins (phasins) were discovered in PHA-accumulating bacteria. They play a crucial role as a structural protein during initial PHA-granule formation and granule growth and also serve as interfaces for granule stabilization in vivo. The phasin PhaP{sub Ah} from Aeromonas hydrophila strain 4AK4 was crystallized using the hanging-drop vapour-diffusion method. Single crystals were cryocooled for X-ray diffraction analysis. The phasin crystals belonged to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 80.8, b = 108.9, c = 134.4 Å.

Growth and characterization of a new nonlinear optical organic crystal: 2,4,6-Trimethylacetanilide

NASA Astrophysics Data System (ADS)

Upadhyaya, V.; Prabhu, Sharada G.

2015-09-01

A new nonlinear optical organic material, 2,4,6-trimethylacetanilide (246TMAA), also known as N-[2,4,6- trimethylphenyl]acetamide, has been synthesized and grown as a single crystal by the slow evaporation technique by organic solvents. The grown crystals have been characterized by morphology study. The crystals are prismatic. Surface examination shows granular dendritic pattern in optical micrograph. The Scanning Electron Micrograph shows the layered growth of the crystal. The Differential Scanning Calorimeter plot shows no phase change until melting point (219°C). The density of the crystals is 1.1g/cc and the crystals are soft. The crystals are transparent in the visible region and in the ultra-violet region till 280 nm. 246TMAA crystallizes with 2 molecules in a monoclinic unit cell in the noncentrosymmetric point group m, space group Pn. Refractive indices of this optically biaxial crystal along the three crystallophysical axes have been measured at 633 nm. The optical second harmonic generation efficiency of the crystal at 1064 nm is about half that of the urea crystal, measured by powder method using Nd:YAG laser. The results show that the 246TMAA crystal can efficiently be used for up-conversion of infrared radiation into visible green light. The powder X-ray diffraction spectrum of the crystal has been obtained.

Growth of NH4Cl Single Crystal from Vapor Phase in Vertical Furnace

NASA Astrophysics Data System (ADS)

Nigara, Yutaka; Yoshizawa, Masahito; Fujimura, Tadao

1983-02-01

A pure and internally stress-free single crystal of NH4Cl was grown successfully from the vapor phase. The crystal measured 1.6 cmφ× 2 cm and had the disordered CsCl structure, which was stable below 184°C. The crystal was grown in an ampoule in a vertical furnace, in which the vapor was efficiently transported both by diffusion and convection. In line with the growth mechanism of a single crystal, the temperature fluctuation (°C/min) on the growth interface was kept smaller than the product of the temperature gradient (°C/cm) and the growth rate (cm/min). The specific heat of the crystal was measured around -31°C (242 K) during cooling and heating cycles by AC calorimetry. The thermal hysteresis (0.4 K) obtained here was smaller than that (0.89 K) of an NH4Cl crystal grown from its aqueous solution with urea added as a habit modifier.

Supramolecular network through Nsbnd H…O, Osbnd H…O and Csbnd H…O hydrogen bonding interaction and density functional theory studies of 4-methylanilinium-3-carboxy-4-hydroxybenzenesulphonate crystal

NASA Astrophysics Data System (ADS)

Rajkumar, M.; Muthuraja, P.; Dhandapani, M.; Chandramohan, A.

2018-02-01

By utilizing the hydrogen bonding strategy, 4-methylanilinium-3-hydroxy-4-corboxy-benzenesulphonate (4MABS), an organic proton transfer molecular salt was synthesized and single crystals of it were successfully grown by slow solvent evaporation solution growth technique at ambient temperature. The 1H and 13C NMR spectra were recorded to establish the molecular structure of the title salt. The single crystal XRD analysis reveals that the title salt crystallizes in monoclinic crystal system with centrosymmetric space group, P21/n. Further, the title salt involves extensive intermolecular Nsbnd H…O, Osbnd H…O and Csbnd H…O as well as intramolecular Osbnd H…O hydrogen bonding interactions to construct supramolecular architecture. All quantum chemical calculations were performed at the level of density functional theory (DFT) with B3LYP functional using 6-311G (d,p) basis atomic set. The photoluminescence spectrum was recorded to explore the emission property of the title crystal. The presence of the various vibrational modes and functional groups in the synthesized salt was confirmed by FT-IR studies. The thermal behaviour of title crystal was established employing TG/DTA analyses. The mechanical properties of the grown crystal were determined by Vicker's microhardness studies. Dielectric measurements were carried out on the grown crystal at a different temperature to evaluate electrical properties.

Cloning, purification, crystallization and preliminary crystallographic analysis of SecA from Enterococcus faecalis

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

Meining, Winfried, E-mail: wim@csb.ki.se; Scheuring, Johannes; Fischer, Markus

2006-06-01

SecA ATPase from E. faecalis has been cloned, overexpressed, purified and crystallized. Crystals belong to space group C2 and diffract to 2.4 Å resolution. The gene coding for SecA from Enterococcus faecalis was cloned and overexpressed in Escherichia coli. In this protein, the lysine at position 6 was replaced by an asparagine in order to reduce sensitivity towards proteases. The modified protein was purified and crystallized. Crystals diffracting to 2.4 Å resolution were obtained using the vapour-diffusion technique. The crystals belong to the monoclinic space group C2, with unit-cell parameters a = 203.4, b = 49.8, c = 100.8 Å,more » α = γ = 90.0, β = 119.1°. A selenomethionine derivative was prepared and is currently being tested in crystallization trials.« less

Crystallization and preliminary X-ray diffraction study of the protealysin precursor belonging to the peptidase family M4

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

Gromova, T. Yu., E-mail: duk@img.ras.ru; Demidyuk, I. V.; Kostrov, S. V.

2008-09-15

A protealysin precursor (the enzyme of the peptidase family M4) was crystallized for the first time. The crystal-growth conditions were found, and single crystals of the protein with dimensions of 0.3-0.5 mm were grown. The preliminary X-ray diffraction study of the enzyme was performed. The protealysin precursor was shown to crystallize in two crystal modifications suitable for the X-ray diffraction study of the three-dimensional structure of the protein molecule at atomic resolution.

Optimization of the crystal growth of the superconductor CaKFe4As4 from solution in the FeAs -CaFe2As2-KFe2As2 system

NASA Astrophysics Data System (ADS)

Meier, W. R.; Kong, T.; Bud'ko, S. L.; Canfield, P. C.

2017-06-01

Measurements of the anisotropic properties of single crystals play a crucial role in probing the physics of new materials. Determining a growth protocol that yields suitable high-quality single crystals can be particularly challenging for multicomponent compounds. Here we present a case study of how we refined a procedure to grow single crystals of CaKFe4As4 from a high temperature, quaternary liquid solution rich in iron and arsenic ("FeAs self-flux"). Temperature dependent resistance and magnetization measurements are emphasized, in addition to the x-ray diffraction, to detect intergrown CaKFe4As4 , CaFe2As2 , and KFe2As2 within what appear to be single crystals. Guided by the rules of phase equilibria and these data, we adjusted growth parameters to suppress formation of the impurity phases. The resulting optimized procedure yielded phase-pure single crystals of CaKFe4As4 . This optimization process offers insight into the growth of quaternary compounds and a glimpse of the four-component phase diagram in the pseudoternary FeAs -CaFe2As2-KFe2As2 system.

Enhanced superconductivity at the interface of W/Sr2RuO4 point contact

NASA Astrophysics Data System (ADS)

Wei, Jian; Wang, He; Lou, Weijian; Luo, Jiawei; Liu, Ying; Ortmann, J. E.; Mao, Z. Q.

Differential resistance measurements are conducted for point contacts (PCs) between the Sr2RuO4 (SRO) single crystal and the tungsten tip. Since the tungsten tip is hard enough to penetrate through the surface layer, consistent superconducting features are observed. Firstly, with the tip pushed towards the crystal, the zero bias conductance peak (ZBCP) due to Andreev reflection at the normal-superconducting interface increases from 3% to more than 20%, much larger than previously reported, and extends to temperature higher than the bulk transition temperature. Reproducible ZBCP within 0.2 mV may also help determine the gap value of SRO, on which no consensus has been reached. Secondly, the logarithmic background can be fitted with the Altshuler-Aronov theory of electron-electron interaction for tunneling into quasi two dimensional electron system. Feasibility of such fitting confirms that spectroscopic information like density of states is probed, and electronic temperature retrieved from such fitting can be important to analyse the PC spectra. Third, at bias much higher than 0.2 mV there are conductance dips due to the critical current effect and these dips persist up to 6.2 K. For more details see. National Basic Research Program of China (973 Program) through Grant No. 2011CBA00106 and No. 2012CB927400.

Direct detection of density of gap states in C60 single crystals by photoemission spectroscopy

NASA Astrophysics Data System (ADS)

Bussolotti, Fabio; Yang, Janpeng; Hiramoto, Masahiro; Kaji, Toshihiko; Kera, Satoshi; Ueno, Nobuo

2015-09-01

We report on the direct and quantitative evaluation of density of gap states (DOGS) in large-size C60 single crystals by using ultralow-background, high-sensitivity ultraviolet photoemission spectroscopy. The charging of the crystals during photoionization was overcome using photoconduction induced by simultaneous laser irradiation. By comparison with the spectra of as-deposited and gas exposed C60 thin films the following results were found: (i) The DOGS near the highest occupied molecular orbital edge in the C60 single crystals (1019-1021states e V-1c m-3) mainly originates from the exposure to inert and ambient gas atmosphere during the sample preparation, storage, and transfer; (ii) the contribution of other sources of gap states such as structural imperfections at grain boundaries is negligible (<1018states e V-1c m-3) .

Improving axion detection sensitivity in high purity germanium detector based experiments

NASA Astrophysics Data System (ADS)

Xu, Wenqin; Elliott, Steven

2015-04-01

Thanks to their excellent energy resolution and low energy threshold, high purity germanium (HPGe) crystals are widely used in low background experiments searching for neutrinoless double beta decay, e.g. the MAJORANA DEMONSTRATOR and the GERDA experiments, and low mass dark matter, e.g. the CDMS and the EDELWEISS experiments. A particularly interesting candidate for low mass dark matter is the axion, which arises from the Peccei-Quinn solution to the strong CP problem and has been searched for in many experiments. Due to axion-photon coupling, the postulated solar axions could coherently convert to photons via the Primakeoff effect in periodic crystal lattices, such as those found in HPGe crystals. The conversion rate depends on the angle between axions and crystal lattices, so the knowledge of HPGe crystal axis is important. In this talk, we will present our efforts to improve the HPGe experimental sensitivity to axions by considering the axis orientations in multiple HPGe crystals simultaneously. We acknowledge the support of the U.S. Department of Energy through the LANL/LDRD Program.

Heat capacity, resistivity, and angular dependent magnetization studies of single crystal Nd 1 + ϵ Fe 4 B 4 for ϵ ≈ 1 7

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

Conner, Benjamin S.; Susner, Michael A.; UES Inc., Beavercreek, OH

Advances in crystal growth have allowed for synthesis of large single crystals of Nd 1+ϵFe 4B 4, a well-known phase with a modulated structure. As a result we are able to report heat capacity and resistivity measurements on a single crystal Nd 1+ϵFe 4B 4 sample with a distribution of ϵ that skews towards the solubility limit of Nd near ϵ ≈ 17. Heat capacity measurements show evidence of crystal field splitting at temperatures higher than the long-range ferromagnetic Curie temperature. Heat capacity, resistivity, and magnetization measurements all confirm a Curie temperature of 7 K which is lower than previouslymore » reported values in the Nd 1+ϵFe 4B 4 system. Here, we also perform measurements of the angular dependence of the magnetization and discover behavior associated with the magnetic anisotropy that is inconsistent with the simple description previously proposed.« less

Heat capacity, resistivity, and angular dependent magnetization studies of single crystal Nd 1 + ϵ Fe 4 B 4 for ϵ ≈ 1 7

DOE PAGES

Conner, Benjamin S.; Susner, Michael A.; UES Inc., Beavercreek, OH; ...

2017-04-04

Advances in crystal growth have allowed for synthesis of large single crystals of Nd 1+ϵFe 4B 4, a well-known phase with a modulated structure. As a result we are able to report heat capacity and resistivity measurements on a single crystal Nd 1+ϵFe 4B 4 sample with a distribution of ϵ that skews towards the solubility limit of Nd near ϵ ≈ 17. Heat capacity measurements show evidence of crystal field splitting at temperatures higher than the long-range ferromagnetic Curie temperature. Heat capacity, resistivity, and magnetization measurements all confirm a Curie temperature of 7 K which is lower than previouslymore » reported values in the Nd 1+ϵFe 4B 4 system. Here, we also perform measurements of the angular dependence of the magnetization and discover behavior associated with the magnetic anisotropy that is inconsistent with the simple description previously proposed.« 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.

An intra-cavity pumped dual-wavelength laser operating at 946 nm and 1064 nm with Nd:YAG  +  Nd:YVO4 crystals

NASA Astrophysics Data System (ADS)

He-Dong, Xiao; Yuan, Dong; Yu, Liu; Shu-Tao, Li; Yong-Ji, Yu; Guang-Yong, Jin

2016-09-01

We adopt a compact intra-cavity pumped structure of Nd:YAG and Nd:YVO4 crystals to develop an efficient dual-wavelength laser that operates at 946 nm and 1064 nm. A 808 nm laser diode is used to pump the Nd:YAG crystal, which emits at 946 nm, and the Nd:YVO4 crystal, which emits at 1064 nm, is intra-cavity pumped at 946 nm. In order to avoid unnecessary pump light passing though the Nd:YAG crystal, reaching the Nd:YVO4 crystal and having an impact on the cavity pump, the two crystals are placed as far from one another as possible in this experiment. The output power at 1064 nm can be adjusted from 1 W-2.9 W by varying the separation between the two crystals. A total output power of 4 W at the dual-wavelengths is achieved at an incident pump power of 30.5 W, where the individual output powers for the 946 nm and 1064 nm emissions are 1.1 W and 2.9 W, respectively.

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.

Crystallization, X-ray diffraction analysis and SIRAS/molecular-replacenent phasing of three crystal forms of Anabaena sensory rhodopsin transducer

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

Vogeley, Lutz; Luecke, Hartmut, E-mail: hudel@uci.edu

2006-04-01

Crystals of Anabaena sensory rhodopsin transducer, the transducer for the cyanobacterial photosensor Anabaena sensory rhodopsin, obtained in the space groups P4, C2 and P2{sub 1}2{sub 1}2{sub 1} diffract to 1.8, 2.1 and 2.0 Å, respectively. Phases for these crystal forms were obtained by SIRAS phasing using an iodide quick-soak derivative (P4) and molecular replacement (C2 and P2{sub 1}2{sub 1}2{sub 1}). Anabaena sensory rhodopsin transducer (ASRT) is a 14.7 kDa soluble signaling protein associated with the membrane-embedded light receptor Anabaena sensory rhodopsin (ASR) from Anabaena sp., a freshwater cyanobacterium. Crystals of ASRT were obtained in three different space groups, P4, C2more » and P2{sub 1}2{sub 1}2{sub 1}, which diffract to 1.8, 2.1 and 2.0 Å, respectively. Phases for one of these crystal forms (P4) were obtained by SIRAS phasing using an iodide quick-soak derivative and a partial model was built. Phases for the remaining crystal forms were obtained by molecular replacement using the partial model from the P4 crystal form.« less

Phase transition studied by 7Li nuclear magnetic resonance in LiXSO4 (X = K, Rb, Cs and NH4) single crystals

NASA Astrophysics Data System (ADS)

Lim, Ae Ran; Choh, Sung Ho; Jeong, Se-Young

2000-11-01

The temperature dependences of 7Li nuclear magnetic resonance in LiXSO4 (X = K, Rb, Cs, and NH4) single crystals grown by the slow evaporation method have been investigated by employing a Bruker FT NMR spectrometer. From the experimental data, the nuclear quadrupole constant, the asymmetry parameter and the principal axes of the EFG tensor were determined, and the results were compared with the crystal structure. The temperature dependences of the quadrupole parameters were explained with a single torsional mode of the Li-O bond by the Bayer theory. All the LiO4 tetrahedra in four different crystals showed torsional motion about the X-axis of the EFG tensor. Based on these results, the differences in atomic weight of X in the LiXSO4 single crystals are responsible for the differences in the torsional angular frequencies.

Order and disorder in crystals of hexameric NTPases from dsRNA bacteriophages.

PubMed

Mancini, Erika J; Grimes, Jonathan M; Malby, Robyn; Sutton, Geoffrey C; Kainov, Denis E; Juuti, Jarmo T; Makeyev, Eugene V; Tuma, Roman; Bamford, Dennis H; Stuart, David I

2003-12-01

The packaging of genomic RNA in members of the Cystoviridae is performed by P4, a hexameric protein with NTPase activity. Across family members such as Phi6, Phi8 and Phi13, the P4 proteins show low levels of sequence identity, but presumably have similar atomic structures. Initial structure-determination efforts for P4 from Phi6 and Phi8 were hampered by difficulties in obtaining crystals that gave ordered diffraction. Diffraction from crystals of full-length P4 showed a variety of disorder and anisotropy. Subsequently, crystals of Phi13 P4 were obtained which yielded well ordered diffraction to 1.7 A. Comparison of the packing arrangements of P4 hexamers in different crystal forms and analysis of the disorder provides insights into the flexibility of this family of proteins, which might be an integral part of their biological function.

Kyropoulos method for growth of nonlinear optical organic crystal ABP (4-aminobenzophenone) from the melt

NASA Astrophysics Data System (ADS)

Pan, Shoukui; Okano, Y.; Tsunekawa, S.; Fukuda, T.

1993-03-01

The Kyropoulus method was used to grow nonlinear optical organic crystals ABP (4-aminobenzophenone). The crystals were characterized by nonlinear optical measurements and had a large effect of frequency doubling.

Phase behavior and crystal structure of 3-(1-naphthyloxy)- and 3-(4-indolyloxy)-propane-1,2-diol, synthetic precursors of chiral drugs propranolol and pindolol

NASA Astrophysics Data System (ADS)

Bredikhin, Alexander A.; Gubaidullin, Aidar T.; Bredikhina, Zemfira A.; Fayzullin, Robert R.; Samigullina, Aida I.; Zakharychev, Dmitry V.

2013-08-01

Valuable precursors of popular chiral drugs propranolol and pindolol, 3-(1-naphthyloxy)-propane-1,2-diol 3 and 3-(4-indolyloxy)-propane-1,2-diol 4 were investigated by IR spectroscopy, DSC, and X-ray diffraction methods. Both compounds, crystallizing from enantiopure feed material, form "guaifenesin-like" crystal packing in which the classic H-bonded bilayers, framed in both sides by hydrophobic fragments of the molecules, acts as the basic crystal-forming motif. Diol 4 prone to spontaneous resolution and conserves its packing pattern crystallizing from racemate. Under the same conditions, diol 3 forms weakly stable solid racemic compound. Some reasons for such a behavior are identified and discussed.

Laser performance of in-band pumped Er : LiYF4 and Er : LiLuF4 crystals

NASA Astrophysics Data System (ADS)

Gorbachenya, K. N.; Kurilchik, S. V.; Kisel, V. E.; Yasukevich, A. S.; Kuleshov, N. V.; Nizamutdinov, A. S.; Korableva, S. L.; Semashko, V. V.

2016-02-01

Spectroscopic properties of Er : LiLuF4 and Er : LiYF4 crystals in the spectral region near 1.5 μm and the lasing characteristics of these crystals under in-band pumping at a wavelength of 1522 nm are studied. With the Er : LiLuF4 crystal, the maximum slope efficiency with respect to the absorbed pump power was 44% at a wavelength of 1609 nm. Continuous-wave operation of an inband pumped Er : LiYF4 laser is obtained for the first time. The output power at a wavelength of 1606 nm was 58 mW with a slope efficiency of 21%.

Influence of pH and method of crystallization on the solid physical form of indomethacin.

PubMed

Dubbini, Alessandra; Censi, Roberta; Martena, Valentina; Hoti, Ela; Ricciutelli, Massimo; Malaj, Ledjan; Di Martino, Piera

2014-10-01

The purpose of this study was to investigate the effect of pH and method of crystallization on the solid physical form of indomethacin (IDM). IDM, a non steroidal anti-inflammatory drug poorly soluble in water, underwent two different crystallization methods: crystallization by solvent evaporation under reduced pressure at 50.0°C (method A), and crystallization by cooling of solution from 50.0 to 5.0°C (method B). In both cases, several aqueous ethanolic solutions of IDM of different pHs were prepared. pHs were adjusted by adding acidic solutions (HCl 2M) or alkali (NaOH or NH4OH 2M) to an aqueous ethanolic solution of IDM. Thus, several batches were recovered after crystallization. The chemical stability of IDM was verified through (1)H NMR and mass spectroscopy (FIA-ESI-MS), that revealed that IDM degraded in strong alkali media (pH ≥ 12). Crystals obtained under different crystallization conditions at pHs of 1.0, 4.5, 7.0, 8.0, 10.0 and chemically stable were thus characterized for crystal habit by scanning electron microscopy, for thermal behaviour by differential scanning calorimetry, and thermogravimetry, and for solid state by X-ray powder diffractometry. Under the Method A, IDM always crystallized into pure metastable alpha form when solutions were acidified or alkalized respectively with HCl and NH4OH. On the contrary, in presence of NaOH, IDM crystallized under a mixture of alpha and sodium trihydrate form, because the presence of the sodium counter ion orientates the crystallization towards the formation of the trihydrate salt. Under the method B, at pH of 1.0, IDM crystallized under the alpha form; at pH 4.5, IDM crystallized under the form alpha in presence of some nuclei of gamma form; at pH 7.0, 8.0, and 10.0 for NH4OH, IDM crystallized under the most stable polymorph gamma form, whereas in presence of NaOH, a mix of alpha, and salt forms was formed whatever the pH of the solution. Copyright © 2014 Elsevier B.V. All rights reserved.

Science Notes.

ERIC Educational Resources Information Center

School Science Review, 1985

1985-01-01

Presents 23 experiments, activities, field projects and computer programs in the biological and physical sciences. Instructional procedures, experimental designs, materials, and background information are suggested. Topics include fluid mechanics, electricity, crystals, arthropods, limpets, acid neutralization, and software evaluation. (ML)

Proton-induced radioactivity in NaI (Tl) scintillation detectors

NASA Technical Reports Server (NTRS)

Fishman, G. J.

1977-01-01

Radioactivity induced by protons in sodium iodide scintillation crystals were calculated and directly measured. These data are useful in determining trapped radiation and cosmic-ray induced, background-counting rates in spaceborne detectors.

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

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

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

2015-01-15

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

Black-on-white polymer-stabilized cholesteric formulations

NASA Astrophysics Data System (ADS)

West, John L.; Magyar, Gregory R.; Francl, James J.; Nixon, Christine M.

1995-08-01

Recent research by Doane, Yang, and Chien demonstrated the use of cholesteric liquid crystals in multiplexed, high resolution, reflective diplays. These materials utilize the bistability of the cholesteric planar and focal conic states for displays with a colored image on a black background. Many commercial applications of these materials, such as electronic books and newspapers, portable faxes and personal data assistants, require, or at least prefer, black-on- white images. We report on relatively high polymer content (equalsV 20% by weight) dispersions of cholesteric liquid crystals that produce a white, reflecting, planar state. The polymer network appears to form cholesteric domains with varying pitch lengths resulting in planar states that reflect in the red, green, and blue portions of the spectrum. Utilizing a black absorbing layer behind a display using these materials offers white images on a black background, or vice-versa.

Simulation of Laser Induced Thermal Damage in Nd:YVO4 Crystals

NASA Astrophysics Data System (ADS)

Nagi, Richie

Neodymium-doped yttrium orthovanadate (Nd:YVO4) is a commonly used gain medium in Diode Pumped Solid State (DPSS) lasers, but high heat loading of Nd:YVO4 at high pump powers (≥ 5 W) leads to thermal distortions and crystal fracture, which limits the utility of Nd:YVO 4 for high power applications. In this thesis, a Nd:YVO4 crystal suffered thermal damage during experiments for investigating the optical gain characteristics of the crystal. This thesis examines the thermal damage mechanisms in detail. Principally, laser induced melting, as well as laser induced thermal stress fracture were studied, all in the absence of stimulated emission in the crystal. The optical system for coupling the pump laser light into the crystal was first simulated in Zemax, an optical design software, and the simulations were then compared to the experimental coupling efficiency results, which were found to be in agreement. The simulations for the laser coupling system were then used in conjunction with LASCAD, a finite element analysis software, to obtain the temperatures inside the crystal, as a function of optical power coupled into the crystal. The temperature simulations were then compared to the experimental results, which were in excellent agreement, and the temperature simulations were then generalized to other crystal geometries and Nd doping levels. Zemax and LASCAD were also used to simulate the thermal stress in the crystal as a function of the coupled optical power, and the simulations were compared to experiments, both of which were found to be in agreement. The thermal stress simulations were then generalized to different crystal geometries and Nd doping levels as well.

Crystal structures and intermolecular interactions of two novel antioxidant triazolyl-benzimidazole compounds

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

Karayel, A., E-mail: matchlessjimmy@163.com, E-mail: yccaoh@hotmail.com; Özbey, S.; Ayhan-Kılcıgil, G.

2015-12-15

The crystal structures of 5-(2-(p-chlorophenylbenzimidazol-1-yl-methyl)-4-(3-fluorophenyl)-2, 4-dihydro-[1,2,4]-triazole-3-thione (G6C) and 5-(2-(p-chlorophenylbenzimidazol-1-yl-methyl)-4-(2-methylphenyl)-2, 4-dihydro-[1,2,4]-triazole-3-thione (G4C) have been determined by single-crystal X-ray diffraction. Benzimidazole ring systems in both molecules are planar. The triazole part is almost perpendicular to the phenyl and the benzimidazole parts of the molecules in order to avoid steric interactions between the rings. The crystal structures are stabilized by intermolecular hydrogen bonds between the amino group of the triazole and the nitrogen atom of benzimidazole of a neighboring molecule.

Proposed square spiral microfabrication architecture for large three-dimensional photonic band gap crystals.

PubMed

Toader, O; John, S

2001-05-11

We present a blueprint for a three-dimensional photonic band gap (PBG) material that is amenable to large-scale microfabrication on the optical scale using glancing angle deposition methods. The proposed chiral crystal consists of square spiral posts on a tetragonal lattice. In the case of silicon posts in air (direct structure), the full PBG can be as large as 15% of the gap center frequency, whereas for air posts in a silicon background (inverted structure) the maximum PBG is 24% of the center frequency. This PBG occurs between the fourth and fifth bands of the photon dispersion relation and is very robust to variations (disorder) in the geometrical parameters of the crystal.

Gamma-ray background induced by atmospheric neutrons

NASA Astrophysics Data System (ADS)

Ma, Y.-Q.

1984-03-01

A small piggyback detector system is used to study the reduction of gamma-ray background induced by atmospheric neutrons in the type of actively shielded gamma-ray spectroscopes. The system consists of two 1.5 x 1.5 arcsec NaI crystal units, one of which is surrounded by some neutron shield material. The results of a balloon flight in 1981 are presented. The data show that a shield of 3 cm-thick pure paraffin cannot reduce the gamma-ray background. On the contrary, it may even cause some enhancement.

Synthesis, growth, structural, optical, luminescence, surface and HOMO LUMO analysis of 2-[2-(4-cholro-phenyl)-vinyl]-1-methylquinolinium naphthalene-2-sulfonate organic single crystals grown by a slow evaporation technique

NASA Astrophysics Data System (ADS)

Karthigha, S.; Kalainathan, S.; Maheswara Rao, Kunda Uma; Hamada, Fumio; Yamada, Manabu; Kondo, Yoshihiko

2016-02-01

Single crystals of 2-[2-(4-cholro-phenyl)-vinyl]-1-methylquinolinium naphthalene-2-sulfonate (4CLNS) were grown by a slow evaporation technique. The formation of molecule was confirmed from 1H NMR and FTIR analysis. The confirmation of crystal structure was done by single crystal XRD and atomic packing of grown crystal was identified. The grown single crystal crystallized in triclinic structure with centrosymmetric space group P-1. The crystalline nature of the synthesised material was recorded by powder XRD. The optical absorption properties of the grown crystals were analyzed by UV-vis spectral studies. The thermal behaviour of the title material has been studied by TG/DTA analysis which revealed the stability of the compound till its melting point 276.7 °C. The third order nonlinear optical property of 4CLNS was investigated in detail by Z scan technique and it confirms that the title crystal is suitable for photonic devices and NLO optical applications. Emissions at 519 nm in green region of the EM spectrum were found by photoluminescence studies. The charge transfer occurring within the molecule is explained by the calculated HOMO and LUMO energies.

An approach to crystallizing proteins by metal-mediated synthetic symmetrization

PubMed Central

Laganowsky, Arthur; Zhao, Minglei; Soriaga, Angela B; Sawaya, Michael R; Cascio, Duilio; Yeates, Todd O

2011-01-01

Combining the concepts of synthetic symmetrization with the approach of engineering metal-binding sites, we have developed a new crystallization methodology termed metal-mediated synthetic symmetrization. In this method, pairs of histidine or cysteine mutations are introduced on the surface of target proteins, generating crystal lattice contacts or oligomeric assemblies upon coordination with metal. Metal-mediated synthetic symmetrization greatly expands the packing and oligomeric assembly possibilities of target proteins, thereby increasing the chances of growing diffraction-quality crystals. To demonstrate this method, we designed various T4 lysozyme (T4L) and maltose-binding protein (MBP) mutants and cocrystallized them with one of three metal ions: copper (Cu2+), nickel (Ni2+), or zinc (Zn2+). The approach resulted in 16 new crystal structures—eight for T4L and eight for MBP—displaying a variety of oligomeric assemblies and packing modes, representing in total 13 new and distinct crystal forms for these proteins. We discuss the potential utility of the method for crystallizing target proteins of unknown structure by engineering in pairs of histidine or cysteine residues. As an alternate strategy, we propose that the varied crystallization-prone forms of T4L or MBP engineered in this work could be used as crystallization chaperones, by fusing them genetically to target proteins of interest. PMID:21898649

Yb7Ni4InGe12: a quaternary compound having mixed valent Yb atoms grown from indium flux.

PubMed

Subbarao, Udumula; Jana, Rajkumar; Chondroudi, Maria; Balasubramanian, Mahalingam; Kanatzidis, Mercouri G; Peter, Sebastian C

2015-03-28

The new intermetallic compound Yb7Ni4InGe12 was obtained as large silver needle shaped single crystals from reactive indium flux. Single crystal X-ray diffraction suggests that Yb7Ni4InGe12 crystallizes in the Yb7Co4InGe12 structure type, and tetragonal space group P4/m and lattice constants are a = b = 10.291(2) Å and c = 4.1460(8) Å. The crystal structure of Yb7Ni4InGe12 consists of columnar units of three different types of channels filled with the Yb atoms. The crystal structure of Yb7Ni4InGe12 is closely related to Yb5Ni4Ge10. The effective magnetic moment obtained from the magnetic susceptibility measurements in the temperature range 200-300 K is 3.66μB/Yb suggests mixed/intermediate valence behavior of ytterbium atoms. X-ray absorption near edge spectroscopy (XANES) confirms that Yb7Ni4InGe12 exhibits mixed valence.

Crystal and molecular structure of 2,6-dibromo-3-chloro-4-fluoroaniline

NASA Astrophysics Data System (ADS)

Betz, R.

2015-12-01

The crystal and molecular structure of 2,6-dibromo-3-chloro-4-fluoroaniline is determined. The crystals are monoclinic, a = 3.8380(3), b = 13.1010(12), c = 8.0980(8) Å, β = 96.010(4)°, V = 404.94(6) Å3, Z = 2, sp. gr. P21. Classical intra- and intermolecular hydrogen bonds of the N-H··· Hal type are observed next to a series of dispersive halogen···halogen interactions in the crystal structure.

Linearly polarized pumped passively Q-switched Nd:YVO4 microchip laser for Ince-Gaussian laser modes with controllable orientations

NASA Astrophysics Data System (ADS)

He, Hong-Sen; Zhang, Ming-Ming; Dong, Jun; Ueda, Ken-Ichi

2016-12-01

A tilted, linearly polarized laser diode end-pumped Cr4+:YAG passively Q-switched a-cut Nd:YVO4 microchip laser for generating numerous Ince-Gaussian (IG) laser modes with controllable orientations has been demonstrated by selecting the crystalline orientation of an a-cut Nd:YVO4 crystal. The same IG laser mode with different orientations has been achieved with the same absorbed pump power in a passively Q-switched Nd:YVO4 microchip laser under linearly polarized pumping when the incident pump power and the crystalline orientation of an a-cut Nd:YVO4 crystal are both properly selected. The significant improvement of pulsed laser performance of controllable IG modes has been achieved by selecting the crystalline orientation of an a-cut Nd:YVO4 crystal. The maximum pulse energy is obtained along the a-axis of an a-cut Nd:YVO4 crystal and the highest peak power is achieved along the c-axis of an a-cut Nd:YVO4 crystal, respectively, which has potential applications on quantum computation and optical manipulation. The generation of controllable IG laser modes in microchip lasers under linearly polarized pumping provides a convenient and universal way to control IG laser mode numbers with anisotropic crystal as a gain medium.

ICESat-2 laser Nd:YVO4 amplifier

NASA Astrophysics Data System (ADS)

Sawruk, Nicholas W.; Burns, Patrick M.; Edwards, Ryan E.; Litvinovitch, Viatcheslav; Martin, Nigel; Witt, Greg; Fakhoury, Elias; Iskander, John; Pronko, Mark S.; Troupaki, Elisavet; Bay, Michael M.; He, Charles C.; Wang, Liqin L.; Cavanaugh, John F.; Farrokh, Babak; Salem, Jonathan A.; Baker, Eric

2018-02-01

We report on the cause and corrective actions of three amplifier crystal fractures in the space-qualified laser systems used in NASA Goddard Space Flight Center's (GSFC) Ice, Cloud, and Land Elevation Satellite-2 (ICESat-2). The ICESat-2 lasers each contain three end-pumped Nd:YVOO4 amplifier stages. The crystals are clamped between two gold plated copper heat spreaders with an indium foil thermal interface material, and the crystal fractures occurred after multiple years of storage and over a year of operational run-time. The primary contributors are high compressive loading of the NdYVO4 crystals at the beginning of life, a time dependent crystal stress caused by an intermetallic reaction of the gold plating and indium, and slow crack growth resulting in a reduction in crystal strength over time. An updated crystal mounting scheme was designed, analyzed, fabricated and tested. Thee fracture slab failure analysis, finite-element modeling and corrective actions are presented.

Synthesis, characterization and single crystal x-ray analysis of a complex of iron(II) bis(2,4-dimethylphenyl)dithiophosphate with 4-ethylpyridine

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

Kumar, Sandeep; Andotra, Savit; Kaur, Mandeep

2016-09-15

Complex of iron(II) bis(2,4-dimethylphenyl)dithiophosphate with 4-ethylpyridine [((2,4- (CH{sub 3}){sub 2}C{sub 6}H{sub 3}O)2PS2)2Fe(NC{sub 5}H{sub 4}(C{sub 2}H{sub 5})-4){sub 2}] is synthesized and characterized by elemental analysis, magnetic moment, IR spectroscopy and single crystal X-ray analysis. Complex crystallizes in the monoclinic sp. gr. P2{sub 1}/n, Z = 2. Crystal structure consists of mononuclear units with Fe(II) ion chelated by four S atoms of the two diphenyldithiophosphate ligands in bidentate manner. N atoms from two 4-ethylpyridine ligands are axially coordinated to the Fe(II) atom leading to an octahedral geometry.

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

NASA Astrophysics Data System (ADS)

Saravanan, M.

2016-08-01

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

Purification, crystallization and preliminary X-ray analysis of a thermostable glycoside hydrolase family 43 β-xylosidase from Geobacillus thermoleovorans IT-08

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

Rohman, Ali; Oosterwijk, Niels van; Kralj, Slavko

2007-11-01

The β-xylosidase was crystallized using PEG 6000 as precipitant. 5% PEG 6000 yielded bipyramid-shaped tetragonal crystals diffracting to 1.55 Å resolution, and 13% PEG 6000 gave rectangular monoclinic crystals diffracting to 1.80 Å resolution. The main enzymes involved in xylan-backbone hydrolysis are endo-1,4-β-xylanase and β-xylosidase. β-Xylosidase converts the xylo-oligosaccharides produced by endo-1,4-β-xylanase into xylose monomers. The β-xylosidase from the thermophilic Geobacillus thermoleovorans IT-08, a member of glycoside hydrolase family 43, was crystallized at room temperature using the hanging-drop vapour-diffusion method. Two crystal forms were observed. Bipyramid-shaped crystals belonging to space group P4{sub 3}2{sub 1}2, with unit-cell parameters a = bmore » = 62.53, c = 277.4 Å diffracted to 1.55 Å resolution. The rectangular crystals belonged to space group P2{sub 1}, with unit-cell parameters a = 57.94, b = 142.1, c = 153.9 Å, β = 90.5°, and diffracted to 1.80 Å resolution.« less

A Cultural Resources Survey of the Proposed Recreational Development Areas and Wildlife Subimpoundments at the B. Everett Jordan Dam and Lake. Volume 1.

DTIC Science & Technology

1984-03-01

containing flow banding, light-gray felsite, felsic- porphyries , crystal tuffs, and rare mafic porphyries and crystal tuffs (Conley and Bain 1965:12Z). The...goods are also present in the form of glass beads, gunflints, iron axes, copper hawk bells and white clay trade pipes. HISTORICAL BACKGROUND The...points manufactured on two rock types occur most frequently: andesitic felsite in the lower valley and grey latite porphyry in the upper valley. The

Pump beam waist-dependent pulse energy generation in Nd:YAG/Cr4+:YAG passively Q-switched microchip laser

NASA Astrophysics Data System (ADS)

Li, Chao-yu; Dong, Jun

2016-08-01

The incident pump beam waist-dependent pulse energy generation in Nd:YAG/Cr4+:YAG composite crystal passively Q-switched microchip laser has been investigated experimentally and theoretically by moving the Nd:YAG/Cr4+:YAG composite crystal along the pump beam direction. Highest pulse energy of 0.4 mJ has been generated when the Nd:YAG/Cr4+:YAG composite crystal is moved about 6 mm away from the focused pump beam waist. Laser pulses with pulse width of 1.7 ns and peak power of over 235 kW have been achieved. The theoretically calculated effective laser beam area at different positions of Nd:YAG/Cr4+:YAG composite crystal along the pump beam direction is in good agreement with the experimental results. The highest peak power can be generated by adjusting the pump beam waist incident on the Nd:YAG/Cr4+:YAG composite crystal to optimize the effective laser beam area in passively Q-switched microchip laser.

Zn3Sb4O6F6: Hydrothermal synthesis, crystal structure and nonlinear optical properties

NASA Astrophysics Data System (ADS)

Ali, Sk Imran; Zhang, Weiguo; Halasyamani, P. Shiv; Johnsson, Mats

2017-12-01

Zn3Sb4O6F6 has been synthesized hydrothermally at 230 °C. The crystal structure was determined from single crystal X-ray diffraction data. It crystallizes in the cubic non-centrosymmetric space group I-43m with the unit cell parameter a = 8.1291(4) Å and is isostructural with M3Sb4O6F6 (M = Co, Ni). The new compound is the first oxofluoride containing Zn2+ and a p-element cation with a stereochemically active lone pair. The crystal structure is made up by [ZnO2F4] octahedra forming a network via corner sharing at F-atoms and [SbO3] trigonal pyramids that form [Sb4O6] cages that connect via the O-atoms to the Zn-atoms. Powder second-harmonic generation (SHG) measurements using 1064 nm radiation on Zn3Sb4O6F6 indicate an SHG intensity of approximately 40 × α-SiO2.

Structure of Cs{sub 4}(HSO{sub 4}){sub 3}(H{sub 2}PO{sub 4}) single crystals

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

Makarova, I. P., E-mail: makarova@crys.ras.ru; Grebenev, V. V.; Vasil’ev, I. I.

2016-01-15

Single crystals of Cs{sub 4}(HSO{sub 4}){sub 3}(H{sub 2}PO{sub 4}) are synthesized and studied for the first time. The new compound is found in the course of studies of the phase diagram of the CsHSO{sub 4}–CsH{sub 2}PO{sub 4}–H{sub 2}O triple system. Data on the atomic crystal structure of single-crystalline and powder specimens, as well as on structural phase transitions, are obtained.

Ytterbium- and neodymium-doped vanadate laser hose crystals having the apatite crystal structure

DOEpatents

Payne, Stephen A.; Kway, Wayne L.; DeLoach, Laura D.; Krupke, William F.; Chai, Bruce H. T.

1994-01-01

Yb.sup.3+ and Nd.sup.3+ doped Sr.sub.5 (VO.sub.4).sub.3 F crystals serve as useful infrared laser media that exhibit low thresholds of oscillation and high slope efficiencies, and can be grown with high optical quality. These laser media possess unusually high absorption and emission cross sections, which provide the crystals with the ability to generate greater gain for a given amount of pump power. Many related crystals such as Sr.sub.5 (VO.sub.4).sub.3 F crystals doped with other rare earths, transition metals, or actinides, as well as the many structural analogs of Sr.sub.5 (VO.sub.4).sub.3 F, where the Sr.sup.2+ and F.sup.- ions are replaced by related chemical species, have similar properties.

Spatial resolution of a hard x-ray CCD detector.

PubMed

Seely, John F; Pereira, Nino R; Weber, Bruce V; Schumer, Joseph W; Apruzese, John P; Hudson, Lawrence T; Szabo, Csilla I; Boyer, Craig N; Skirlo, Scott

2010-08-10

The spatial resolution of an x-ray CCD detector was determined from the widths of the tungsten x-ray lines in the spectrum formed by a crystal spectrometer in the 58 to 70 keV energy range. The detector had 20 microm pixel, 1700 by 1200 pixel format, and a CsI x-ray conversion scintillator. The spectral lines from a megavolt x-ray generator were focused on the spectrometer's Rowland circle by a curved transmission crystal. The line shapes were Lorentzian with an average width after removal of the natural and instrumental line widths of 95 microm (4.75 pixels). A high spatial frequency background, primarily resulting from scattered gamma rays, was removed from the spectral image by Fourier analysis. The spectral lines, having low spatial frequency in the direction perpendicular to the dispersion, were enhanced by partially removing the Lorentzian line shape and by fitting Lorentzian curves to broad unresolved spectral features. This demonstrates the ability to improve the spectral resolution of hard x-ray spectra that are recorded by a CCD detector with well-characterized intrinsic spatial resolution.

President Gerald Ford holds crystal manufactured in space during Skylab 4

NASA Technical Reports Server (NTRS)

1974-01-01

President Gerald R. Ford, center, holds encased crystal manufactured in space during Skylab 4. Dr. James C. Fletcher, left, NASA Administrator, explains the article to the Chief Executive as Dr. Harold Johnson of M.I.T. looks on. The indium-antimonide crystal was formed in Earth orbit on January 6, 1974, by the Skylab 4 astronauts.

Synthesis and NLO studies of novel (2E)-1-(2-bromo-4,5-dimethoxyphenyL)-3-(3-Bromo-4-Fluorophenyl)Prop-2-en-1-one single crystal

NASA Astrophysics Data System (ADS)

Shruthi, C.; Ravindrachary, V.; Prasad, D. Jagadeesh; Guruswamy, B.; Hegde, Shreedatta

2017-05-01

A novel organic nonlinear optical (NLO) material (2E)-1-(2-Bromo-4,5-Dimethoxyphenyl)-3-(3-Bromo-4-Fluorophenyl)Prop-2-en-1-one has been synthesized using Claisen-Schmidth condensation method. The chemical structure of the compound was confirmed by recording its FT-IR spectrum and the functional groups were identified. Single crystals were grown by slow evaporation method and the single crystal XRD study reveals that the compound crystallizes in the monoclinic crystal system with a space group -P 2yn. The observed cell parameters are a = 9.346(5) A°, b = 12.953(7) A°, c = 14.355(8) A°, α = 90°, β = 108.379°(9), γ = 90°. UV-Visible study shows that the compound is transparent in the entire visible region and the absorption takes place in the UV range. The Non linear optical efficiency of the crystal was estimated and it is found to be 0.5 times that of standard KDP crystal.

Crystallization and preliminary X-ray crystallographic analysis of latent isoform PPO4 mushroom (Agaricus bisporus) tyrosinase

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

Mauracher, Stephan Gerhard; Molitor, Christian; Al-Oweini, Rami

Polyphenol oxidase 4 (PPO4) from the natural source A. bisporus was crystallized in its latent precursor form (pro-tyrosinase; Ser2–Thr565) using the 6-tungstotellurate(VI) salt Na{sub 6}[TeW{sub 6}O{sub 24}]·22H{sub 2}O as a crystallization additive. Tyrosinase exhibits catalytic activity for the ortho-hydroxylation of monophenols to diphenols as well as their subsequent oxidation to quinones. Owing to polymerization of these quinones, brown-coloured high-molecular-weight compounds called melanins are generated. The latent precursor form of polyphenol oxidase 4, one of the six tyrosinase isoforms from Agaricus bisporus, was purified to homogeneity and crystallized. The obtained crystals belonged to space group C121 (two molecules per asymmetric unit)more » and diffracted to 2.78 Å resolution. The protein only formed crystals under low-salt conditions using the 6-tungstotellurate(VI) salt Na{sub 6}[TeW{sub 6}O{sub 24}]·22H{sub 2}O as a co-crystallization agent.« less

Test of a prototype neutron spectrometer based on diamond detectors in a fast reactor

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

Osipenko, M.; Ripani, M.; Ricco, G.

2015-07-01

A prototype of neutron spectrometer based on diamond detectors has been developed. This prototype consists of a {sup 6}Li neutron converter sandwiched between two CVD diamond crystals. The radiation hardness of the diamond crystals makes it suitable for applications in low power research reactors, while a low sensitivity to gamma rays and low leakage current of the detector permit to reach good energy resolution. A fast coincidence between two crystals is used to reject background. The detector was read out using two different electronic chains connected to it by a few meters of cable. The first chain was based onmore » conventional charge-sensitive amplifiers, the other used a custom fast charge amplifier developed for this purpose. The prototype has been tested at various neutron sources and showed its practicability. In particular, the detector was calibrated in a TRIGA thermal reactor (LENA laboratory, University of Pavia) with neutron fluxes of 10{sup 8} n/cm{sup 2}s and at the 3 MeV D-D monochromatic neutron source named FNG (ENEA, Rome) with neutron fluxes of 10{sup 6} n/cm{sup 2}s. The neutron spectrum measurement was performed at the TAPIRO fast research reactor (ENEA, Casaccia) with fluxes of 10{sup 9} n/cm{sup 2}s. The obtained spectra were compared to Monte Carlo simulations, modeling detector response with MCNP and Geant4. (authors)« less

Design of a micromachined terahertz electromagnetic crystals (EMXT) channel-drop filter on silicon-substrate

NASA Astrophysics Data System (ADS)

Zhou, Kai; Liu, Yong; Si, Liming; Lv, Xin

2013-08-01

An integrated 0.5 THz electromagnetic crystals(EMXT) channel-drop filter based on PBG structure is presented in this paper. A channel-drop filter is a device in which a narrow bandwidth is redirected to another "drop" waveguide while other frequencies are unaffected. It's capable of extracting a certain frequency from a continuous spectrum in the bus channel and passing it to the test channel. It has potential applications in photonic integrated circuits, radio astronomy, THz spectroscopy, THz communication and remote sensing radar receiver. PBG structures(or photonic crystals) are periodic structures which possess band gaps, where the electromagnetic wave of certain ranges of frequencies cannot pass through and is reflected. The proposed channel-drop filter consists of input waveguide,output waveguide and PBG structure. The proposed filter is simulated using the finite element method and can be fabricated by micro-electromechanical systems (MEMS) technology,due to its low cost, high performance and high processing precision.The filter operation principle and fabrication process are discussed.The simulation results show its ability to filter the frequency of 496GHz with a linewidth of approximately 4GHz and transmission of 27.2 dB above background.The loss at resonant frequency is less than 1dB considering the thickness and roughness of gold layer required by the MEMS process.The channel drop efficiency is 84%.

The Crystal Zero Degree Detector at BESIII

NASA Astrophysics Data System (ADS)

Koch, L.; Denig, A.; Drexler, P.; Garillon, B.; Johansson, T.; Kühn, W.; Lange, S.; Lauth, W.; Liang, Y.; Marciniewski, P.; Rathmann, T.; Redmer, C.

2017-07-01

The BESIII experiment at the BEPCII electron positron collider at IHEP (Beijing) is collecting data in the charm-τ mass region. Electron positron collisions are a very well suited environment for the study of initial state radiation (ISR). However, the photons from ISR are strongly peaked towards small polar angles and are currently detected with limited efficiency. In order to increase the detection efficiency of ISR photons, we are developing small-size calorimeters to be placed in the very forward and backward regions. Each detector will consist of two 4×3 arrays of 1×1×14 cm3 LYSO crystals. A 1 cm gap separating each of the two arrays will reduce the contamination from background at very low angles. The scintillation light will be collected by silicon photomultipliers (SiPMs). The expected event rate in the MHz range requires flash ADCs recording the preamplified SiPM outputs.The digitized waveforms will be analyzed in realtime yielding data reduction and pile-up detection. This high bandwidth data stream will be transmitted via optical fibers to FPGA-based hardware performing sub-event building, buffering, and event correlation with the BESIII trigger. The sub-events with a corresponding trigger will be sent to the BESIII event builder via TCP/IP. A single crystal equipped with a SiPM was instrumented as a prototype detector. Tests with radioactive sources were performed successfully.

Factors affecting calcium oxalate dihydrate fragmented calculi regrowth

PubMed Central

Costa-Bauzá, A; Perelló, J; Isern, B; Sanchis, P; Grases, F

2006-01-01

Background The use of extracorporeal shock wave lithotripsy (ESWL) to treat calcium oxalate dihydrate (COD) renal calculi gives excellent fragmentation results. However, the retention of post-ESWL fragments within the kidney remains an important health problem. This study examined the effect of various urinary conditions and crystallization inhibitors on the regrowth of spontaneously-passed post-ESWL COD calculi fragments. Methods Post-ESWL COD calculi fragments were incubated in chambers containing synthetic urine varying in pH and calcium concentration: pH = 5.5 normocalciuria (3.75 mM), pH = 5.5 hypercalciuria (6.25 mM), pH = 6.5 normocalciuria (3.75 mM) or pH = 6.5 hypercalciuria (6.25 mM). Fragment growth was evaluated by measuring increases in weight. Fragment growth was standardized by calculating the relative mass increase. Results Calcium oxalate monohydrate (COM) crystals formed on COD renal calculi fragments under all conditions. Under pH = 5.5 normocalciuria conditions, only COM crystals formed (growth rate = 0.22 ± 0.04 μg/mg·h). Under pH = 5.5 hypercalciuria and under pH = 6.5 normocalciuria conditions, COM crystals and a small number of new COD crystals formed (growth rate = 0.32 ± 0.03 μg/mg·h and 0.35 ± 0.05 μg/mg·h, respectively). Under pH = 6.5 hypercalciuria conditions, large amounts of COD, COM, hydroxyapatite and brushite crystals formed (growth rate = 3.87 ± 0. 34 μg/mg·h). A study of three crystallization inhibitors demonstrated that phytate completely inhibited fragment growth (2.27 μM at pH = 5.5 and 4.55 μM at pH = 6.5, both under hypercalciuria conditions), while 69.0 μM pyrophosphate caused an 87% reduction in mass under pH = 6.5 hypercalciuria conditions. In contrast, 5.29 mM citrate did not inhibit fragment mass increase under pH = 6.5 hypercalciuria conditions. Conclusion The growth rate of COD calculi fragments under pH = 6.5 hypercalciuria conditions was approximately ten times that observed under the other three conditions. This observation suggests COD calculi residual fragments in the kidneys together with hypercalciuria and high urinary pH values may be a risk factor for stone growth. The study also showed the effectiveness of specific crystallization inhibitors in slowing calculi fragment growth. PMID:16822299

Rocks and Minerals.

ERIC Educational Resources Information Center

Naturescope, 1987

1987-01-01

Provides background information on rocks and minerals, including the unique characteristics of each. Teaching activities on rock-hunting and identification, mineral configurations, mystery minerals, and growing crystals are provided. Reproducible worksheets are included for two of the activities. (TW)

Single-Crystal Structure of a Covalent Organic Framework

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

Zhang, YB; Su, J; Furukawa, H

2013-11-06

The crystal structure of a new covalent organic framework, termed COF-320, is determined by single-crystal 3D electron diffraction using the rotation electron diffraction (RED) method for data collection. The COF crystals are prepared by an imine condensation of tetra-(4-anilyl)methane and 4,4'-biphenyldialdehyde in 1,4-dioxane at 120 degrees C to produce a highly porous 9-fold interwoven diamond net. COF-320 exhibits permanent porosity with a Langmuir surface area of 2400 m(2)/g and a methane total uptake of 15.0 wt % (176 cm(3)/cm(3)) at 25 degrees C and 80 bar. The successful determination of the structure of COF-320 directly from single-crystal samples is anmore » important advance in the development of COF chemistry.« less

Detection of bremsstrahlung radiation of 90Sr-90Y for emergency lung counting.

PubMed

Ho, A; Hakmana Witharana, S S; Jonkmans, G; Li, L; Surette, R A; Dubeau, J; Dai, X

2012-09-01

This study explores the possibility of developing a field-deployable (90)Sr detector for rapid lung counting in emergency situations. The detection of beta-emitters (90)Sr and its daughter (90)Y inside the human lung via bremsstrahlung radiation was performed using a 3″ × 3″ NaI(Tl) crystal detector and a polyethylene-encapsulated source to emulate human lung tissue. The simulation results show that this method is a viable technique for detecting (90)Sr with a minimum detectable activity (MDA) of 1.07 × 10(4) Bq, using a realistic dual-shielded detector system in a 0.25-µGy h(-1) background field for a 100-s scan. The MDA is sufficiently sensitive to meet the requirement for emergency lung counting of Type S (90)Sr intake. The experimental data were verified using Monte Carlo calculations, including an estimate for internal bremsstrahlung, and an optimisation of the detector geometry was performed. Optimisations in background reduction techniques and in the electronic acquisition systems are suggested.

Laser performance of in-band pumped Er : LiYF{sub 4} and Er : LiLuF{sub 4} crystals

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

Gorbachenya, K N; Kisel, V E; Yasukevich, A S

2016-02-28

Spectroscopic properties of Er : LiLuF{sub 4} and Er : LiYF{sub 4} crystals in the spectral region near 1.5 μm and the lasing characteristics of these crystals under in-band pumping at a wavelength of 1522 nm are studied. With the Er : LiLuF{sub 4} crystal, the maximum slope efficiency with respect to the absorbed pump power was 44% at a wavelength of 1609 nm. Continuous-wave operation of an inband pumped Er : LiYF{sub 4} laser is obtained for the first time. The output power at a wavelength of 1606 nm was 58 mW with a slope efficiency of 21%. (lasers)

Infrared-active optical phonons in LiFePO4 single crystals

NASA Astrophysics Data System (ADS)

Stanislavchuk, T. N.; Middlemiss, D. S.; Syzdek, J. S.; Janssen, Y.; Basistyy, R.; Sirenko, A. A.; Khalifah, P. G.; Grey, C. P.; Kostecki, R.

2017-07-01

Infrared-active optical phonons were studied in olivine LiFePO4 oriented single crystals by means of both rotating analyzer and rotating compensator spectroscopic ellipsometry in the spectral range between 50 and 1400 cm-1. The eigenfrequencies, oscillator strengths, and broadenings of the phonon modes were determined from fits of the anisotropic harmonic oscillator model to the data. Optical phonons in a heterosite FePO4 crystal were measured from the delithiated ab-surface of the LiFePO4 crystal and compared with the phonon modes of the latter. Good agreement was found between experimental data and the results of solid-state hybrid density functional theory calculations for the phonon modes in both LiFePO4 and FePO4.

Optimization of the crystal growth of the superconductor CaKFe 4 As 4 from solution in the FeAs - CaFe 2 As 2 - KFe 2 As 2 system

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

Meier, W. R.; Kong, T.; Bud'ko, S. L.

Measurements of the anisotropic properties of single crystals play a crucial role in probing the physics of new materials. Determining a growth protocol that yields suitable high-quality single crystals can be particularly challenging for multicomponent compounds. Here we present a case study of how we refined a procedure to grow single crystals of CaKFe 4As 4 from a high temperature, quaternary liquid solution rich in iron and arsenic (“FeAs self-flux”). Temperature dependent resistance and magnetization measurements are emphasized, in addition to the x-ray diffraction, to detect intergrown CaKFe 4As 4, CaFe 2As 2, and KFe 2As 2 within what appearmore » to be single crystals. Guided by the rules of phase equilibria and these data, we adjusted growth parameters to suppress formation of the impurity phases. The resulting optimized procedure yielded phase-pure single crystals of CaKFe 4As 4. In conclusion, this optimization process offers insight into the growth of quaternary compounds and a glimpse of the four-component phase diagram in the pseudoternary FeAs–CaFe 2As 2–KFe 2As 2 system.« less

Optimization of the crystal growth of the superconductor CaKFe 4 As 4 from solution in the FeAs - CaFe 2 As 2 - KFe 2 As 2 system

DOE PAGES

Meier, W. R.; Kong, T.; Bud'ko, S. L.; ...

2017-06-19

Measurements of the anisotropic properties of single crystals play a crucial role in probing the physics of new materials. Determining a growth protocol that yields suitable high-quality single crystals can be particularly challenging for multicomponent compounds. Here we present a case study of how we refined a procedure to grow single crystals of CaKFe 4As 4 from a high temperature, quaternary liquid solution rich in iron and arsenic (“FeAs self-flux”). Temperature dependent resistance and magnetization measurements are emphasized, in addition to the x-ray diffraction, to detect intergrown CaKFe 4As 4, CaFe 2As 2, and KFe 2As 2 within what appearmore » to be single crystals. Guided by the rules of phase equilibria and these data, we adjusted growth parameters to suppress formation of the impurity phases. The resulting optimized procedure yielded phase-pure single crystals of CaKFe 4As 4. In conclusion, this optimization process offers insight into the growth of quaternary compounds and a glimpse of the four-component phase diagram in the pseudoternary FeAs–CaFe 2As 2–KFe 2As 2 system.« less

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

PubMed

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

2018-02-15

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

Performance evaluation for 120 four-layer DOI block detectors of the jPET-D4.

PubMed

Inadama, Naoko; Murayama, Hideo; Ono, Yusuke; Tsuda, Tomoaki; Hamamoto, Manabu; Yamaya, Taiga; Yoshida, Eiji; Shibuya, Kengo; Nishikido, Fumihiko; Takahashi, Kei; Kawai, Hideyuki

2008-01-01

The jPET-D4 is a brain positron emission tomography (PET) scanner that we have developed to meet user demands for high sensitivity and high spatial resolution. For this scanner, we developed a four-layer depth-of-interaction (DOI) detector. The four-layer DOI detector is a key component for the jPET-D4, its performance has great influence on the overall system performance. Previously, we reported the original technique for encoding four-layer DOI. Here, we introduce the final design of the jPET-D4 detector and present the results of an investigation on uniformity in performance of the detector. The performance evaluation was done over the 120 DOI crystal blocks for the detectors, which are to be assembled into the jPET-D4 scanner. We also introduce the crystal assembly method, which is simple enough, even though each DOI crystal block is composed of 1,024 crystal elements. The jPET-D4 detector consists of four layers of 16 x 16 Gd(2)SiO(5) (GSO) crystals and a 256-channel flat-panel position-sensitive photomultiplier tube (256ch FP-PMT). To identify scintillated crystals in the four-layer DOI detector, we use pulse shape discrimination and position discrimination on the two-dimensional (2D) position histogram. For pulse shape discrimination, two kinds of GSO crystals that show different scintillation decay time constants are used in the upper two and lower two layers, respectively. Proper reflector arrangement in the crystal block then allows the scintillated crystals to be identified in these two-layer groupings with two 2D position histograms. We produced the 120 DOI crystal blocks for the jPET-D4 system, and measured their characteristics such as the accuracy of pulse shape discrimination, energy resolution, and the pulse height of the full energy peak. The results show a satisfactory and uniform performance of the four-layer DOI crystal blocks; for example, misidentification rate in each GSO layer is <5% based on pulse shape discrimination, the averaged energy resolutions for the central four crystals of the first (farthest from the FP-PMT), second, third, and 4th layers are 15.7 +/- 1.0, 15.8 +/- 0.6, 17.7 +/- 1.2, and 17.3 +/- 1.4%, respectively, and variation in pulse height of the full energy peak among the four layers is <5% on average.

X-ray diffraction studies of enkephalins. Crystal structure of [(4'-bromo) Phe4,Leu5]enkephalin.

PubMed Central

Ishida, T; Kenmotsu, M; Mino, Y; Inoue, M; Fujiwara, T; Tomita, K; Kimura, T; Sakakibara, S

1984-01-01

In order to investigate the structure-activity relationship of [Leu5]- and [Met5]enkephalins, [(4'-bromo)Phe4, Leu5]-, [(4'-bromo)Phe4, Met5]- and [Met5] enkephalins were synthesized and crystallized. The crystal structure of [(4'-bromo) Phe4, Leu5]- enkephalin was determined by X-ray diffraction method using the heavy atom method and refined to R = 0.092 by the least-squares method. The molecule in this crystal took essentially the same type I' beta-turn conformation found in [Leu5]enkephalin [Smith & Griffin (1978) Science 199, 1214-1216). On the other hand, the preliminary three-dimensional Patterson analyses showed that the most probable conformations of [(4'-bromo)Phe4,Met5]- and [Met5]enkephalins are both the dimeric extended forms. Based on these insights, the biologically active conformation of enkephalin was discussed in relation to the mu- and delta-receptors. PMID:6721829

New crystals of the CsHSO{sub 4}–CsH{sub 2}PO{sub 4}–H{sub 2}O system

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

Makarova, I. P., E-mail: makarova@crys.ras.ru; Grebenev, V. V.; Komornikov, V. A.

2016-11-15

Cs{sub 6}H(HSO{sub 4}){sub 3}(H{sub 2}PO{sub 4}){sub 4} crystals, grown for the first time based on an analysis of the phase diagram of the CsHSO{sub 4}–CsH{sub 2}PO{sub 4}–H{sub 2}O ternary system, have been investigated by structural analysis using synchrotron radiation. The atomic structure of the crystals is determined and its specific features are analyzed.

Studies on the growth aspects, structural, thermal, dielectric and third order nonlinear optical properties of solution grown 4-methylpyridinium p-nitrophenolate single crystal

NASA Astrophysics Data System (ADS)

Devi, S. Reena; Kalaiyarasi, S.; Zahid, I. MD.; Kumar, R. Mohan

2016-11-01

An ionic organic optical crystal of 4-methylpyridinium p-nitrophenolate was grown from methanol by slow evaporation method at ambient temperature. Powder and single crystal X-ray diffraction studies revealed the crystal system and its crystalline perfection. The rocking curve recorded from HRXRD study confirmed the crystal quality. FTIR spectral analysis confirmed the functional groups present in the title compound. UV-visible spectral study revealed the optical window and band gap of grown crystal. The thermal, electrical and surface laser damage threshold properties of harvested crystal were examined by using TGA/DTA, LCR/Impedance Analyzer and Nd:YAG laser system respectively. The third order nonlinear optical property of grown crystal was elucidated by Z-scan technique.

Crystallization of lysozyme with ( R)-, ( S)- and ( RS)-2-methyl-2,4-pentanediol

DOE PAGES

Stauber, Mark; Jakoncic, Jean; Berger, Jacob; ...

2015-03-01

Chiral control of crystallization has ample precedent in the small-molecule world, but relatively little is known about the role of chirality in protein crystallization. In this study, lysozyme was crystallized in the presence of the chiral additive 2-methyl-2,4-pentanediol (MPD) separately using the R and S enantiomers as well as with a racemic RS mixture. Crystals grown with ( R)-MPD had the most order and produced the highest resolution protein structures. This result is consistent with the observation that in the crystals grown with ( R)-MPD and ( RS)-MPD the crystal contacts are made by ( R)-MPD, demonstrating that there ismore » preferential interaction between lysozyme and this enantiomer. These findings suggest that chiral interactions are important in protein crystallization.« less

Study of the growth and pyroelectric properties of TGS crystals doped with aniline-family dipolar molecules

NASA Astrophysics Data System (ADS)

Zhang, Kecong; Song, Jiancheng; Wang, Min; Fang, Changshui; Lu, Mengkai

1987-04-01

TGS crystals doped with aniline-family dipolar molecules (aniline, 2-aminobenzoic acid, 3-aminobenzoic acid, 3-aminobenzene-sulphonic acid, 4-aminobenzenesulphonic acid and 4-nitroraniline) have been grown by the slow-cooling solution method. The influence of these dopants on the growth habits, crystal morphology pyroelectric properties, and structure parameters of TGS crystals has been systematically investigated. The effects of the domain structure of the seed crystal on the pyroelectric properties of the doped crystals have been studied. It is found that the spontaneous polarization (P), pyroelectric coefficient (lambda), and internal bias field of the doped crystals are slightly higher than those of the pure TGS, and the larger the dipole moment of the dopant molecule, the higher the P and lambda of the doped TGS crystal.

Synthesis, growth, structural, spectral, thermal, chemical etching, linear and nonlinear optical and mechanical studies of an organic single crystal 4-chloro 4-nitrostilbene (CONS): a potential NLO material.

PubMed

Dinakaran, Paul M; Kalainathan, S

2013-07-01

4-Chloro 4-nitrostilbene (CONS) a new organic nonlinear optical material has been synthesized. Employing slow evaporation method, good optical quality single crystals (dimensions up to 6×2×3 mm(3)) have been grown using ethyl methyl ketone (EMK) as a solvent. The grown crystals have been subjected to various characterizations such as single crystal X-ray diffraction, powder XRD, Fourier Transform Infrared spectroscopy (FTIR), proton NMR, solid UV absorption, SHG studies. Single crystal X-ray diffraction reveals that the crystal system belongs to monoclinic with noncentrosymmetric space group P21. The UV-Vis absorption spectrum has been recorded and found that the cut off wavelength is 380 nm. Functional groups and the structure of the title compound have been confirmed by FTIR and (1)H NMR spectroscopic analyses respectively. Molecular mass of the CONS confirmed by the high resolution mass spectral analysis .The thermal behavior of the grown crystal has been studied by TG/DTA analysis and it shows the melting point is at 188.66 °C. Dislocations and growth pattern present in the grown crystal revealed by the etching study. The mechanical strength of the CONS crystal has been studied by Vicker's hardness measurement. The SHG efficiency of the grown crystal has been determined by Kurtz and Perry powder test which revealed that the CONS crystal (327 mV) has 15 times greater efficiency than that of KDP (21.7 mV). Copyright © 2013 Elsevier B.V. All rights reserved.

Simplifying the growth of hybrid single-crystals by using nanoparticle precursors: the case of AgI

NASA Astrophysics Data System (ADS)

Xu, Biao; Wang, Ruji; Wang, Xun

2012-03-01

We report the synthesis of a series of AAgmIn single-crystals within 24 h, at room temperature, utilizing AgI nanoparticles (NPs) as the precursor. The AgI NPs impart high reactivity under mild conditions and favor the growth kinetics. 0D, 1D and 2D iodoargentate crystals can be obtained. This work represents the first application of NPs in the field of organo-metal-halide crystals and will inspire the design of other AMmXn crystals.We report the synthesis of a series of AAgmIn single-crystals within 24 h, at room temperature, utilizing AgI nanoparticles (NPs) as the precursor. The AgI NPs impart high reactivity under mild conditions and favor the growth kinetics. 0D, 1D and 2D iodoargentate crystals can be obtained. This work represents the first application of NPs in the field of organo-metal-halide crystals and will inspire the design of other AMmXn crystals. Electronic supplementary information (ESI) available: XPS spectra of AgI NPs, schematic representation of the formation process of [Ag4I8]4- in 2, UV-Vis spectra of the DTMA-Ag-I clusters, analysis of force balance of a crystal at the interface between H2O and CH2Cl2 and crystal structure depiction of 1-4. CIF files of 1-4 are also provided. CCDC reference numbers 863848, 863849, 863850 and 863851. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c2nr30139c

Synthesis, growth, structural, optical, spectral, thermal and mechanical studies of 4-methoxy 4-nitrostilbene (MONS): a new organic nonlinear optical single crystal.

PubMed

Dinakaran, Paul M; Bhagavannarayana, G; Kalainathan, S

2012-11-01

4-Methoxy 4-nitrostilbene (MONS), a new organic nonlinear optical material has been synthesized. Based on the solubility data good quality single crystal with dimensions up to 38×11×3 mm(3) has been grown by slow evaporation method using ethyl methyl ketone (MEK) as a solvent. Powder XRD confirms the crystalline property and also the diffraction planes have been indexed. The lattice parameters for the grown MONS crystals were determined by using single crystal X-ray diffraction analysis and it reveals that the crystal lattice system is triclinic. The crystalline perfection of the grown crystals has been analysed by high resolution X-ray diffraction (HRXRD) rocking curve measurements. Fourier transform infrared (FTIR) spectrum for powdered MONS sample confirms the functional groups present in the grown crystal. The UV-vis absorption spectrum has been recorded in the range of 190-1100 nm and the cut off wavelength 499 nm has been determined. The optical constants of MONS have been determined through UV-vis-NIR spectroscopy. The MONS crystals were further subjected to other characterizations. i.e., (1)H NMR, TG/DTA, photoluminescence and microhardness test. The Kurtz and Perry powder technique confirms the NLO property of the grown crystal and the SHG efficiency of MONS was found to be 1.55× greater than that of KDP crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis, crystal structure and antioxidant evaluation of C-4-acetamidophenylcalix[4]pyrogallolarene

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

Abosadiya, Hamza M.; Hasbullah, Siti Aishah; Yamin, Bohari M.

2015-09-25

C-4-acetamidophenylcalix[4]pyrogallolarene was synthesized by an acid catalyzed condensation reaction of pyrogallol with 4-acetamidobenzaldehyde. The compound was characterized by IR, {sup 1}H and {sup 13}C NMR spectroscopy. Single crystal X-ray analysis revealed that the molecule crystallized in a triclinic system with space group Pī and the unit cell dimensions a= 12.2948(16) Å, b= 13.4423(17) Å, c= 13.5906(18) Å, α =107.549(4)°, β =102.034(4)°, γ =90.535(4)°, Z= 1 and V= 2088.2(5) Å{sup 3}. The macrocyclic calix adopts a chair (C{sub 2h}) conformation and the molecule is associated with eight DMSO molecules of crystallization. Antioxidant test by DPPH method showed that the compound exhibitsmore » good antioxidant activity of about 72%.« less

Crystal structure and density of helium to 232 kbar

NASA Technical Reports Server (NTRS)

Mao, H. K.; Wu, Y.; Jephcoat, A. P.; Hemley, R. J.; Bell, P. M.; Bassett, W. A.

1988-01-01

The properties of helium and hydrogen at high pressure are topics of great interest to the understanding of planetary interiors. These materials constitute 95 percent of the entire solar system. A technique was presented for the measurement of X-ray diffraction from single-crystals of low-Z condenses gases in a diamond-anvil cell at high pressure. The first such single-crystal X-ray diffraction measurements on solid hydrogen to 26.5 GPa were presented. The application of this technique to the problem of the crystal structure, equation of state, and phase diagram of solid helium is reported. Crucial for X-ray diffraction studies of these materials is the use of a synchrotron radiation source which provides high brillance, narrow collimation of the incident and diffracted X-ray beams to reduce the background noise, and energy-dispersive diffraction techniques with polychromatic (white) radiation, which provides high detection efficiency.

Crystal structure and vibrational spectra of piperazinium bis(4-hydroxybenzenesulphonate) molecular-ionic crystal

NASA Astrophysics Data System (ADS)

Marchewka, M. K.; Pietraszko, A.

2008-02-01

The piperazinium bis(4-hydroxybenzenesulphonate) crystallizes from water solution at room temperature in P2 1/ c space group of monoclinic system. The crystals are built up of doubly protonated piperazinium cations and ionized 4-hydroxybenzenesulphonate anions that interact through weak hydrogen bonds of O-H⋯O and N-H⋯O type. Mutual orientation of anions is determined by non-conventional hydrogen bonds of C-H⋯π type. Room temperature powder FT IR and FT Raman measurements were carried out. The vibrational spectra are in full agreement with the structure obtained from X-ray crystallography. The big single crystals of the title salt can be grown.

Preparation, structural characterization, and decomposition studies of two new γ-octamolybdates of 4-methylpyridine.

PubMed

Szymańska, Anna; Nitek, Wojciech; Rutkowska-Zbik, Dorota; Łasocha, Wiesław

We synthesized two new γ-octamolybdates, and determined their crystal structures from single-crystal X-ray diffraction data. Orange-yellow tetrakis(4-methylpyridinium) bis(4-methylpyridine)-γ-octamolybdate 1 crystallizes in space group P2 1 /c with a  = 11.586(2) Å, b  = 15.526(2) Å, c  = 16.247(2) Å, β  = 118.753(1)º, Z  = 2. White tetrakis(4-methylpyridinium) bis(4-methylpyridine)-γ-octamolybdate hydrate 2 crystallizes in space group C2/c with a  = 27.086(4) Å, b  = 11.917(2) Å, c  = 19.332(2) Å, β  = 124.427(1)º, Z  = 4. Results of crystal structure determinations are presented and discussed in this paper. Thermal stability and decomposition studies of the obtained two new γ-octamolybdates were performed using TG/DSC and XRPD methods. Both compounds decomposed with the formation of 4-methylpyridinium β-octamolybdate. The two compounds are pseudo-polymorphs, exhibiting both striking similarities as well as significant differences in their structures and properties.

New crystal forms of Diocleinae lectins in the presence of different dimannosides

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

Moreno, Frederico Bruno Mendes Batista; Bezerra, Gustavo Arruda; Oliveira, Taianá Maia de

2006-11-01

The crystallization and preliminary X-ray data of Canavalia gladiata lectin (CGL) and C. maritima lectin (CML) complexed with Man(α1-2)Man(α1)OMe, Man(α1-3)Man(α1)OMe and Man(α1-4)Man(α1)OMe in two crystal forms [the complexes with Man(α1-3)Man(α1)OMe and Man(α1-4)Man(α1)OMe crystallized in space group P3{sub 2} and those with Man(α1-2)Man(α1)OMe crystallized in space group I222], which differed from those of the native proteins (P2{sub 1}2{sub 1}2 for CML and C222 for CGL), are reported. Studying the interactions between lectins and sugars is important in order to explain the differences observed in the biological activities presented by the highly similar proteins of the Diocleinae subtribe. Here, the crystallization andmore » preliminary X-ray data of Canavalia gladiata lectin (CGL) and C. maritima lectin (CML) complexed with Man(α1-2)Man(α1)OMe, Man(α1-3)Man(α1)OMe and Man(α1-4)Man(α1)OMe in two crystal forms [the complexes with Man(α1-3)Man(α1)OMe and Man(α1-4)Man(α1)OMe crystallized in space group P3{sub 2} and those with Man(α1-2)Man(α1)OMe crystallized in space group I222], which differed from those of the native proteins (P2{sub 1}2{sub 1}2 for CML and C222 for CGL), are reported. The crystal complexes of ConA-like lectins with Man(α1-4)Man(α1)OMe are reported here for the first time.« less

Hematin crystallization from aqueous and organic solvents

NASA Astrophysics Data System (ADS)

Ketchum, Megan A.; Olafson, Katy N.; Petrova, Elena V.; Rimer, Jeffrey D.; Vekilov, Peter G.

2013-09-01

Hematin crystallization is the main mechanism of detoxification of heme that is released in malaria-infected erythrocytes as a byproduct of the hemoglobin catabolism by the parasite. A controversy exists over whether hematin crystals grow from the aqueous medium of the parasite's digestive vacuole or in the lipid bodies present in the vacuole. To this end, we compare the basic thermodynamic and structural features of hematin crystallization in an aqueous buffer at pH 4.8, as in the digestive vacuole, and in water-saturated octanol that mimics the environment of the lipid nanospheres. We show that in aqueous solutions, hematin aggregation into mesoscopic disordered clusters is insignificant. We determine the solubility of the β-hematin crystals in the pH range 4.8-7.6. We image by atomic force microscopy crystals grown at pH 4.8 and show that their macroscopic and mesoscopic morphology features are incompatible with those reported for biological hemozoin. In contrast, crystals grown in the presence of octanol are very similar to those extracted from parasites. We determine the hematin solubility in water-saturated octanol at three temperatures. These solubilities are four orders of magnitude higher than that at pH 4.8, providing for faster crystallization from organic than from aqueous solvents. These observations further suggest that the lipid bodies play a role in mediating biological hemozoin crystal growth to ensure faster heme detoxification.

Thermal, spectroscopic properties and laser performance at 1.06 and 1.33 μm of Nd : Ca 4YO(BO 3) 3 and Nd : Ca 4GdO(BO 3) 3 crystals

NASA Astrophysics Data System (ADS)

Wang, Changqing; Zhang, Huaijin; Meng, Xianlin; Zhu, Li; Chow, Y. T.; Liu, Xuesong; Cheng, Ruiping; Yang, Zhaohe; Zhang, Shaojun; Sun, Lianke

2000-11-01

Nd : Ca 4YO(BO 3) 3 (Nd : YCOB) and Nd : Ca 4GdO(BO 3) 3 (Nd : GdCOB) crystals were grown by Czochralski method. Thermal expansion and specific heat of these two crystals were experimentally determined. Their fluorescence spectra were measured within the range from 1000 to 1500 nm. Laser output experiments at 1.06 and 1.33 μm of Nd : YCOB and Nd : GdCOB crystals were performed with a cw Ti : sapphire laser as the pump source.

Gas-liquid reactive crystallization kinetics of 2,4,6-triamino-1,3,5-trinitrobenzene in the semi-batch procedure

NASA Astrophysics Data System (ADS)

Liu, Ruqin; Huang, Ming; Yao, Xiaolu; Chen, Shuang; Wang, Shucun; Suo, Zhirong

2018-06-01

2,4,6-Triamino-1,3,5-trinitrobenzene is the attractive insensitive high energetic material used extensively in the military and civil fields. Combined with the double-films theory, the global gas-liquid chemical reaction kinetics of 2,4,6-triamino-1,3,5-trinitrobenzene was developed by means of the infinitesimal material balance calculation. The raw material concentration and reactive temperature effects on the crystallization of 2,4,6-triamino-1,3,5-trinitrobenzene were investigated by the batch experiments. The reactive crystallization kinetics associated ammonia feeding rate of 2,4,6-triamino-1,3,5-trinitrobenzene, including nucleation as well as crystal growth, was systematically investigated in the heterogonous semi-batch procedure. The nucleation and crystal growth kinetic exponents were estimated by the linear least-squares method. The crystallization kinetic results indicated that nucleation rate strongly increased but liner growth rate decreased with the increasing of ammonia feeding rate. In terms of manufacturing coarse 2,4,6-triamino-1,3,5-trinitrobenzene, it was found that a slow ammonia feeding rate and a low raw material concentration were feasible under the present experimental conditions.

MgAl2O4 spinel refractory as containment liner for high-temperature alkali salt containing environments

DOEpatents

Peascoe-Meisner, Roberta A [Knoxville, TN; Keiser, James R [Oak Ridge, TN; Hemric, James G [Knoxville, TN; Hubbard, Camden R [Oak Ridge, TN; Gorog, J Peter [Kent, WA; Gupta, Amul [Jamestown, NY

2008-10-21

A method includes containing a high-temperature alkali salt containing environment using a refractory containment liner containing MgAl.sub.2O.sub.4 spinel. A method, includes forming a refractory brick containing MgAl.sub.2O.sub.4 spinel having an exterior chill zone defined by substantially columnar crystallization and an interior zone defined by substantially equiaxed crystallization; and removing at least a portion of the exterior chill zone from the refractory brick containing MgAl.sub.2O.sub.4 spinel by scalping the refractory brick containing MgAl.sub.2O.sub.4 spinel to define at least one outer surface having an area of substantially equiaxed crystallization. A product of manufacture includes a refractory brick containing MgAl.sub.2O.sub.4 spinel including an interior zone defined by substantially equiaxed crystallization; and at least one outer surface having an area of substantially equiaxed crystallization.

Undulated oxo-centered layers in PbLn3O4(VO4) (Ln= La and Nd) and relationship with Nd4O4(GeO4)

NASA Astrophysics Data System (ADS)

Colmont, Marie; Mentré, Olivier; Henry, Natacha; Pautrat, Alain; Leclercq, Bastien; Capet, Frédéric; Djelal, Nora; Roussel, Pascal

2018-04-01

Single crystals of PbLa3O4(VO4) have been synthesized using the flux growth technique and characterized by X-ray diffraction. The crystal structure of the tittle phase was solved by charge flipping and refined to R1 = 0.024 (wR2 = 0.031) for 2777 reflections [I>3σ(I)]. The compound is orthorhombic and crystallized in the space group Cmcm: a = 5.8686(6)Å, b = 17.898(2)Å, c = 7.9190(7)Å, V = 831.8(1)Å3, Z = 4. The structure is built on [PbLa3O4]3+ layers with zig-zag cross-sections, surrounded by isolated (VO4)3- tetrahedra. Its crystal structure shows direct relationship with the isoformular Nd4O4(GeO4) compound which crystallized in the primitive non centrosymmetric Pb21m sub-group. Its stability in temperature and under air was checked as well as optical properties. In a second part, lanthanum was substituted by neodymium giving rise to a paramagnet and f→ f electronic excitations superposed to the broad absorption front below 3.05 eV related to the presence of VO4 groups.

Polarized spectral properties and 1.5-1.6 μm laser operation of Er:Sr3Yb2(BO3)4 crystal

NASA Astrophysics Data System (ADS)

Lin, F. L.; Huang, J. H.; Chen, Y. J.; Gong, X. H.; Lin, Y. F.; Luo, Z. D.; Huang, Y. D.

2013-10-01

Undoped and Er3+-doped Sr3Yb2(BO3)4 crystals were grown by the Czochralski method. Room temperature polarized spectral properties of the Er:Sr3Yb2(BO3)4 crystal were investigated. The efficiency of the energy transfer from Yb3+ to Er3+ ions in this crystal was calculated to be about 95%. End-pumped by a diode laser at 970 nm in a hemispherical cavity, a 0.75 W quasi-CW laser at 1.5-1.6 μm with a slope efficiency of 7% and an absorbed pump threshold of 3.8 W was achieved in a 0.5-mm-thick Z-cut crystal glued on a 5-mm-thick pure YAG crystal with UV-curable adhesive.

Fast growth of n-type 4H-SiC bulk crystal by gas-source method

NASA Astrophysics Data System (ADS)

Hoshino, Norihiro; Kamata, Isaho; Tokuda, Yuichiro; Makino, Emi; Kanda, Takahiro; Sugiyama, Naohiro; Kuno, Hironari; Kojima, Jun; Tsuchida, Hidekazu

2017-11-01

Fast growth of n-type 4H-SiC crystals was attempted using a high-temperature gas-source method. High growth rates exceeding 9 mm/h were archived at a seed temperature of 2550 °C, although the formation of macro-step bunching caused doping fluctuation and voids in the grown crystal. We investigated a trade-off between growth-rate enhancement and macro-step formation and how to improve the trade-off. By controlling the growth conditions, the growth of highly nitrogen-doped 4H-SiC crystals without the doping fluctuation and void formation were accomplished under a high growth rate exceeding 3 mm/h, maintaining the density of threading screw dislocations in the same level with the seed crystal. The influence of growth parameters on nitrogen incorporations into grown crystals was also surveyed.

Crystal conversion between metal-organic frameworks with different crystal topologies for efficient crystal design on two-dimensional substrates

NASA Astrophysics Data System (ADS)

Tsuruoka, Takaaki; Inoue, Kohei; Miyanaga, Ayumi; Tobiishi, Kaho; Ohhashi, Takashi; Hata, Manami; Takashima, Yohei; Akamatsu, Kensuke

2018-04-01

Crystal conversion of metal-organic frameworks (MOFs) between different crystal topologies on a polymer substrate has been successfully achieved by localized dissolution of MOF crystals followed by a rapid self-assembly of framework components. Upon addition of the desired organic linkers to the reaction system containing MOF crystals on the substrate, reversible crystal conversion between the [Cu2(btc)3]n and [Cu2(ndc)2(dabco)]n frameworks (btc = 1,3,5-benzene tricarboxylate, ndc = 1,4-naphthalene dicarboxylate, dabco = 1,4-diazabicyclo[2.2.2]octane) could be routinely achieved in high yields. Most surprisingly, in the case of conversion from the [Cu2(ndc)2(dabco)]n to [Cu2(btc)3]n frameworks, the [Cu2(btc)3]n crystals with unique shapes (cuboctahedron and truncated cube) could be prepared using butanol as a reaction medium.

Synthesis, crystal growth, structural and physicochemical studies of novel binary organic complex: 4-chloroaniline-3-hydroxy-4-methoxybenzaldehyde

NASA Astrophysics Data System (ADS)

Sharma, K. P.; Reddi, R. S. B.; Bhattacharya, S.; Rai, R. N.

2012-06-01

The solid-state reaction, which is solvent free and green synthesis, has been adopted to explore the novel compound. The phase diagram of 4-chloroaniline (CA) and 3-hydroxy-4-methoxybenzaldehyde (HMB) system shows the formation of a novel 1:1 molecular complex, and two eutectics on either sides of complex. Thermochemical studies of complex and eutectics have been carried out for various properties such as heat of fusion, entropy of fusion, Jackson's parameters, interfacial energy and excess thermodynamic functions. The formation of molecular complex was also studied by IR, NMR, elemental analysis and UV-Vis absorption spectra. The single crystal of molecular complex was grown and its XRD study confirms the formation of complex and identifies the crystal structure and atomic packing of crystal of complex. Transmission spectra of grown crystal of the complex show 70% transmittance efficiency with cut off wavelength 412 nm. The band gap and refractive index of the crystal of complex have also been studied.

New structure type in the mixed-valent compound YbCu4Ga8.

PubMed

Subbarao, Udumula; Gutmann, Matthias J; Peter, Sebastian C

2013-02-18

The new compound YbCu(4)Ga(8) was obtained as large single crystals in high yield from reactions run in liquid gallium. Preliminary investigations suggest that YbCu(4)Ga(8) crystallizes in the CeMn(4)Al(8) structure type, tetragonal space group I4/mmm, and lattice constants are a = b = 8.6529(4) Å and c = 5.3976(11) Å. However, a detailed single-crystal XRD revealed a tripling of the c axis and crystallizing in a new structure type with lattice constants of a = b = 8.6529(4) Å and c = 15.465(1) Å. The structural model was further confirmed by neutron diffraction measurements on high-quality single crystal. The crystal structure of YbCu(4)Ga(8) is composed of pseudo-Frank-Kasper cages occupying one ytterbium atom in each ring which are shared through the corner along the ab plane, resulting in a three-dimensional network. The magnetic susceptibility of YbCu(4)Ga(8) investigated in the temperature range 2-300 K showed Curie-Weiss law behavior above 100 K, and the experimentally measured magnetic moment indicates mixed-valent ytterbium. Electrical resistivity measurements show the metallic nature of the compound. At low temperatures, variation of ρ as a function of T indicates a possible Fermi-liquid state at low temperatures.

Synthesis, Crystal and Electronic Structures, and Optical Properties of (CH 3NH 3) 2CdX 4 (X = Cl, Br, I)

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

Roccanova, Rachel; Ming, Wenmei; Whiteside, Vincent R.

Here, we report the synthesis, crystal and electronic structures, as well as optical properties of the hybrid organic–inorganic compounds MA 2CdX 4 (MA = CH 3NH 3; X = Cl, Br, I). MA 2CdI 4 is a new compound, whereas, for MA 2CdCl 4 and MA 2CdBr 4, structural investigations have already been conducted but electronic structures and optical properties are reported here for the first time. Single crystals were grown through slow evaporation of MA 2CdX 4 solutions with optimized conditions yielding mm-sized colorless (X = Cl, Br) and pale yellow (X = I) crystals. Single crystal and variablemore » temperature powder X-ray diffraction measurements suggest that MA 2CdCl 4 forms a 2D layered perovskite structure and has two structural transitions at 283 and 173 K. In contrast, MA 2CdBr 4 and MA 2CdI 4 adopt 0D K 2SO 4-derived crystal structures based on isolated CdX 4 tetrahedra and show no phase transitions down to 20 K. The contrasting crystal structures and chemical compositions in the MA 2CdX 4 family impact their air stabilities, investigated for the first time in this work; MA 2CdCl 4 is air-stable, whereas MA 2CdBr 4 and MA 2CdI 4 partially decompose when left in air. Optical absorption measurements suggest that MA 2CdX 4 have large optical band gaps above 3.9 eV. Room temperature photoluminescence spectra of MA 2CdX 4 yield broad peaks in the 375–955 nm range with full width at half-maximum values up to 208 nm. These PL peaks are tentatively assigned to self-trapped excitons in MA 2CdX 4 following the crystal and electronic structure considerations. The bands around the Fermi level have small dispersions, which is indicative of high charge localization with significant exciton binding energies in MA 2CdX 4. On the basis of our combined experimental and computational results, MA 2CdX 4 and related compounds may be of interest for white-light-emitting phosphors and scintillator applications.« less

Synthesis, Crystal and Electronic Structures, and Optical Properties of (CH 3NH 3) 2CdX 4 (X = Cl, Br, I)

DOE PAGES

Roccanova, Rachel; Ming, Wenmei; Whiteside, Vincent R.; ...

2017-11-02

Here, we report the synthesis, crystal and electronic structures, as well as optical properties of the hybrid organic–inorganic compounds MA 2CdX 4 (MA = CH 3NH 3; X = Cl, Br, I). MA 2CdI 4 is a new compound, whereas, for MA 2CdCl 4 and MA 2CdBr 4, structural investigations have already been conducted but electronic structures and optical properties are reported here for the first time. Single crystals were grown through slow evaporation of MA 2CdX 4 solutions with optimized conditions yielding mm-sized colorless (X = Cl, Br) and pale yellow (X = I) crystals. Single crystal and variablemore » temperature powder X-ray diffraction measurements suggest that MA 2CdCl 4 forms a 2D layered perovskite structure and has two structural transitions at 283 and 173 K. In contrast, MA 2CdBr 4 and MA 2CdI 4 adopt 0D K 2SO 4-derived crystal structures based on isolated CdX 4 tetrahedra and show no phase transitions down to 20 K. The contrasting crystal structures and chemical compositions in the MA 2CdX 4 family impact their air stabilities, investigated for the first time in this work; MA 2CdCl 4 is air-stable, whereas MA 2CdBr 4 and MA 2CdI 4 partially decompose when left in air. Optical absorption measurements suggest that MA 2CdX 4 have large optical band gaps above 3.9 eV. Room temperature photoluminescence spectra of MA 2CdX 4 yield broad peaks in the 375–955 nm range with full width at half-maximum values up to 208 nm. These PL peaks are tentatively assigned to self-trapped excitons in MA 2CdX 4 following the crystal and electronic structure considerations. The bands around the Fermi level have small dispersions, which is indicative of high charge localization with significant exciton binding energies in MA 2CdX 4. On the basis of our combined experimental and computational results, MA 2CdX 4 and related compounds may be of interest for white-light-emitting phosphors and scintillator applications.« less

The Growth of Berlinite (AlPO4) Single Crystals.

DTIC Science & Technology

1980-03-01

Solubility of AlPO 4 18 6. Solubility Data of Jahn and Kordes on AlPO4 19 7. AlPO 4 Seed Crystal 23 8. Tem-Pres Hydrothermal Research Unit 25 9...Since the vapor pressure of water rises rapidly with temperature, a closed hydrothermal system was used. In a seeded hydrothermal growth process, the...to investigate the hydrothermal growth of Berlinite (AlPO4 ) to determine the optimum growth conditions for large high quality crystals. Over thirty

Metastable Solution Thermodynamic Properties and Crystal Growth Kinetics

NASA Technical Reports Server (NTRS)

Kim, Soojin; Myerson, Allan S.

1996-01-01

The crystal growth rates of NH4H2PO4, KH2PO4, (NH4)2SO4, KAl(SO4)2 central dot 12H2O, NaCl, and glycine and the nucleation rates of KBr, KCl, NaBr central dot 2H2O, (NH4)2Cl, and (NH4)2SO4 were expressed in terms of the fundamental driving force of crystallization calculated from the activity of supersaturated solutions. The kinetic parameters were compared with those from the commonly used kinetic expression based on the concentration difference. From the viewpoint of thermodynamics, rate expressions based on the chemical potential difference provide accurate kinetic representation over a broad range of supersaturation. The rates estimated using the expression based on the concentration difference coincide with the true rates of crystallization only in the concentration range of low supersaturation and deviate from the true kinetics as the supersaturation increases.

Collinear and vector interaction of light waves in nonlinear optical crystals KTiOPO4("KTP"), Ba2NaNb5O15 ("banana")

NASA Astrophysics Data System (ADS)

Deinekina, N. A.; Korosteleva, I. A.; Kravchenko, O. V.; Faleev, D. S.

2016-11-01

Esents the research results of biaxial crystals with mm2 symmetry class. These crystals were used for determining regularities of nonlinear conversion of broadband optical emission on the basis of collinear and vector light waves interactions of different nature. The quantities of the basis nonlinear optical characteristics of "KTP" (KTiOPO4) and "banana" (Ba2NaNb5O15) crystals were calculated in case of synchronous conversion of broadband emission from the area of 0.8 - 2.8 micron to the visible spectrum of 0.4 - 0.7 micron. The nonlinear optical characteristics of "KTP" crystals are defined by their geometrical structure, the mode of interaction of light waves, and the infra-red spectrum width, that was experimentally confirmed on "KTP" crystal. The quality characteristics β were calculated for the "KTP" crystal. For "banana" crystal the angle of phase synchronism θc changes insignificantly when the observation plane is changed. It can be explained by the fact that the biaxiality of crystal is not strongly expressed, because of the basis refraction indices the conditions nz<=ny≈nx are performed.

In-Situ Crystallization of a Lithium Disilicate Glass--Effect of Pressure on Crystal Growth Rate

NASA Technical Reports Server (NTRS)

Fuss, T.; Ray, C. S.; Lesher, C. E.; Day, D. E.

2006-01-01

Crystallization of a Li2O.2SiO2 (LS2) glass subjected to a uniform hydrostatic pressure of 4.5 GPa and 6 GPa was investigated up to a temperature of 750 C. The density of the compressed glass is about 2% greater at 4.5 GPa than at 1 atm and, depending upon the processing temperature, up to 10% greater at 6 GPa. Crystal growth rates investigated as a function of temperature and pressure show that lithium disilicate crystal growth is an order of magnitude slower at 4.5 GPa than 1 atm resulting in a shift of +45 C (plus or minus 10 C) in the growth rate curve at high pressure compared to 1 atm condition. At 6 GPa lithium disilicate crystallization is suppressed entirely, while a new high pressure lithium metasilicate crystallizes at temperatures 95 C (plus or minus 10 C) higher than those reported for lithium disilicate crystallization at 1 atm. The decrease in crystal growth rate with increasing pressure for lithium disilicate glass up to 750 C is related to an increase in viscosity with pressure associated with fundamental changes in glass structure accommodating densification.

H/D isotopic recognition and temperature effects in IR spectra of hydrogen-bonded cyclic dimers in crystals: 3-Methylcinnamic acid and 4-phenylbutyric acid

NASA Astrophysics Data System (ADS)

Hachuła, Barbara; Jabłońska-Czapla, Magdalena; Flakus, Henryk T.; Nowak, Maria; Kusz, Joachim

2015-01-01

In the present work, the experimental and theoretical study of the nature of the inter-hydrogen bond interactions in two different carboxylic acids, 3-methylcinnamic acid (3MCA) and 4-phenylbutyric acid (4PBA), were reported. The polarized IR spectra of 3MCA and 4PBA crystals were recorded at the frequency ranges of the νOsbnd H and νOsbnd D bands. The spectral properties of 3MCA and 4PBA interpreted with the aid of the calculations based on the "strong-coupling" model. The differences in the spectral properties of the two different dimeric systems in the crystals provide a valuable information about the existence of a direct relationship between the crystal spectral properties in IR and the electronic structure of the molecular systems. In 3MCA crystals strong vibrational exciton interactions favor a "tail-to-head" (TH)-type Davydov coupling widespread via the π-electrons, whereas in 4PBA crystals a weak "through-space" (SS) exciton coupling is responsible for a "side-to-side"-type coupling. The relative contribution of each individual exciton coupling mechanism in IR spectra generation strongly depends on temperature and molecular electronic structure. The H/D isotopic recognition effect, depending on a non-random distribution of protons and deuterons in the crystal hydrogen bridges, was also analyzed.

H/D isotopic recognition and temperature effects in IR spectra of hydrogen-bonded cyclic dimers in crystals: 3-methylcinnamic acid and 4-phenylbutyric acid.

PubMed

Hachuła, Barbara; Jabłońska-Czapla, Magdalena; Flakus, Henryk T; Nowak, Maria; Kusz, Joachim

2015-01-05

In the present work, the experimental and theoretical study of the nature of the inter-hydrogen bond interactions in two different carboxylic acids, 3-methylcinnamic acid (3MCA) and 4-phenylbutyric acid (4PBA), were reported. The polarized IR spectra of 3MCA and 4PBA crystals were recorded at the frequency ranges of the νO-H and νO-D bands. The spectral properties of 3MCA and 4PBA interpreted with the aid of the calculations based on the "strong-coupling" model. The differences in the spectral properties of the two different dimeric systems in the crystals provide a valuable information about the existence of a direct relationship between the crystal spectral properties in IR and the electronic structure of the molecular systems. In 3MCA crystals strong vibrational exciton interactions favor a "tail-to-head" (TH)-type Davydov coupling widespread via the π-electrons, whereas in 4PBA crystals a weak "through-space" (SS) exciton coupling is responsible for a "side-to-side"-type coupling. The relative contribution of each individual exciton coupling mechanism in IR spectra generation strongly depends on temperature and molecular electronic structure. The H/D isotopic recognition effect, depending on a non-random distribution of protons and deuterons in the crystal hydrogen bridges, was also analyzed. Copyright © 2014 Elsevier B.V. All rights reserved.

Structural and optical effects induced by gamma irradiation on NdPO{sub 4}: X-ray diffraction, spectroscopic and luminescence study

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

Sadhasivam, S.; Rajesh, N.P., E-mail: rajeshnp@hotmail.com

2016-02-15

Highlights: • Inorganic NdPO{sub 4} crystal was grown first time using potassium polyphosphate (K{sub 6}P{sub 4}O{sub 13}) flux. • NdPO{sub 4} crystal is insoluble in water, non-hygroscopic and high radiation resistance favoring for actinides host. • Actinide immobilization can be made at 1273 K. • High yield of 1061 nm photon emission. - Abstract: Rare earth orthophosphate (NdPO{sub 4}) monazite single crystals were grown using high temperature flux growth method employing K{sub 6}P{sub 4}O{sub 13} (K{sub 6}) as molten solvent. Their structural parameters were studied using single crystal X-ray diffraction (XRD) method. The grown crystals were examined by SEM andmore » EDX techniques for their homogeniousity and inclusion in the crystals. The influence of gamma irradiation in structural and optical absorption properties were studied by the powder XRD, FTIR and reflectance spectroscopy. The effect of gamma irradiation on luminescence properties was recorded. No significant structural change is observed up to 150 kGy gamma dose. The gamma ray induced charge trap in the crystal was saturated to 40 kGy dose. The luminescence intensity decreases with an increase in the irradiation. The emission of luminescence intensity stabilizes above 40 kGy gamma dose.« less

Spectroscopic characterisation of Er-doped LuVO4 single crystals

NASA Astrophysics Data System (ADS)

Lisiecki, R.; Dominiak-Dzik, G.; Solarz, P.; Strzęp, A.; Ryba-Romanowski, W.; Łukasiewicz, T.

2010-12-01

The LuVO4:Er single crystals were grown by the Czochralski technique. The crystal-field split energy levels of Er3+ ion were derived experimentally employing absorption and emission spectra measured at T=10 K. The Judd-Ofelt phenomenological method was used to estimate intensity parameters, radiative lifetimes and branching ratios of luminescence. The excited state dynamics of the LuVO4:Er systems was investigated and experimental lifetimes of emitting levels were measured. The emission cross section of the 4I13/2→4I15/2 transition in the infrared was calculated by the Füchtbauer-Ladenburg method. The gain cross section, estimated for several inverse-population parameters, allowed us to evaluate a potential laser activity of the LuVO4:Er system at 1.6 μm. Also, the potential range of the optical pumping was assessed based on absorption spectra achieved at the room temperature. The optical losses related to the green up-converted emission, encountered under the 978 nm excitation between 300 and 670 K were indicated and discussed. Spectroscopic peculiarities of the Er3+-doped LuVO4 crystal were discussed in relation to optical properties of the YVO4:Er and GdVO4:Er crystals. Taking into account the high quantum efficiency of the 4I13/2 level, and satisfactory absorption and emission features, the LuVO4:Er crystal can be considered as a promising active material for laser operation near 1.6 μm.

Experimental and computational studies on creatininium 4-nitrobenzoate - An organic proton transfer complex

NASA Astrophysics Data System (ADS)

Thirumurugan, R.; Anitha, K.

2017-10-01

A new organic proton transfer complex of creatininium 4-nitrobenzoate (C4NB) has been synthesized and its single crystals were grown successfully by slow evaporation technique. The grown single crystal was subjected to various characterization techniques like single crystal X-ray diffraction (SCXRD), FTIR, FT-Raman and Kurtz-Perry powder second harmonic generation (SHG). The SCXRD analysis revealed that C4NB was crystallized into orthorhombic crystal system, with noncentrosymmetric (NCS), P212121 space group. The creatininium cation and 4-nitrobenzoate anion were connected through a pair of N__H⋯O hydrogen bonds (N(3)__H(6) ⋯ O(3) (x+1, y, z) and N(2)__H(5) &ctdot O(2) (x-1/2, -y-1/2, -z+2)) and fashioned a R22(8) ring motif. The crystal structure was stabilized by strong N__H⋯O and weak C__H⋯O intermolecular interactions and it was quantitatively analysed by Hirshfeld surface and fingerprint (FP) analysis. FTIR and FT-Raman studies confirmed the vibrational modes of functional groups present in C4NB compound indubitably. SHG efficiency of grown crystal was 4.6 times greater than that of standard potassium dihydrogen phosphate (KDP) material. Moreover, density functional theory (DFT) studies such as Mulliken charge distribution, frontier molecular orbitals (FMOs), molecular electrostatic potential (MEP) map, natural bond orbital analysis (NBO) and first order hyperpolarizability (β0) were calculated to explore the structure-property relationship.

Synthesis, structure and luminescence of novel co-crystals based on bispyridyl-substituted α,β-unsaturated ketones with coformers

NASA Astrophysics Data System (ADS)

Li, Hong-Juan; Wang, Lei; Zhao, Juan-Juan; Sun, Ju-Feng; Sun, Ji-Liang; Wang, Chun-Hua; Hou, Gui-Ge

2015-01-01

Based on 2,6-bis((pyridin-4-yl)methylene)cyclohexanone (A) and N-methyl-3,5-bis((pyridin-4-yl)methylene)-4-piperidone (B) with coformers, three novel macrocyclic co-crystals, (A)ṡ(resorcinol) (1), (A)ṡ(1,3,5-benzenetriol) (2), (B)2ṡ(1,3,5-benzenetriol)2 (3) and three chain co-crystals, (A)ṡ(hydroquinone) (4), (A)ṡ(isophthalic acid) (5), (B)ṡ(isophthalic acid) (6) have been synthesized and structurally characterized by IR, 1H NMR and X-ray crystal structure analysis. Structural analysis indicates that four-component macrocycles in 1-3 are generated from "clip-like" resorcinol templates and building blocks, while 4-6 show infinite H-bonding chains. In addition, the luminescent properties of A, B and 1-6 are investigated primarily in the solid state. Compared with free building blocks, 1-6 are blue-shifted 55-60 nm with decreasing emission intensities in spite of the enhancement in 6. The change of luminescent properties might be caused mainly by incorporation of coformers into co-crystals, including H-bonds, molecular conformations, arranging dispositions and π-π characteristics. It might have potential applications for crystal engineering to construct patentable crystals with interesting luminescent properties.

Growth, spectroscopic properties and laser output of Er : Ca 4YO(BO 3) 3 and Er : Yb : Ca 4YO(BO 3) 3 crystals

NASA Astrophysics Data System (ADS)

Zhang, Huaijin; Meng, Xianlin; Wang, Changqing; Wang, Pu; Zhu, Li; Liu, Xuesong; Dong, Chunming; Yang, Yuyong; Cheng, Ruiping; Dawes, Judith; Piper, Jim; Zhang, Shaojun; Sun, Lianke

2000-09-01

In this paper, Er : Ca 4YO(BO 3) 3 (Er : YCOB) and Er : Yb : Ca 4YO(BO 3) 3 (Er : Yb : YCOB) crystals with large size and excellent quality have been grown by the Czochralski method. The absorption and emission spectra of Er : YCOB and Er : Yb : YCOB crystals have been measured; the emission spectrum of Er : Yb : YCOB crystal shows that the strongest emission peak is located at 1537 nm. An output power of about 2 mW at the wavelength of 1553 nm has been obtained under the pumping power of a fiber-coupled laser diode (LD) of 1600 mW at 976 nm, using a Y direction cut 2.5 mm thick Er : Yb : YCOB crystal sample.

Crystal Structure of Two V-shaped Ligands with N-Heterocycles

NASA Astrophysics Data System (ADS)

Wang, Gao-Feng; Sun, Shu-Wen; Zhang, Xiao; Sun, Shu-Gang

2017-12-01

Two V-shaped ligands with N-heterocycles, bis(4-(1 H-imidazol-1-yl) phenyl)methanone ( 1), and bis(4-(1 H-benzo[d]imidazol-1-yl)phenyl)methanone ( 2) have been synthesized and characterized by elemental analyses, IR and 1 H NMR spectroscopy. Crystal structures of 1 and 2 have been determined by X-ray diffraction. The crystal of 1 is monoclinic, sp. gr. P21/ c, Z = 4. The crystal of 2 is orthorhombic, sp. gr. Fdd2, Z = 8. X-ray diffraction analyses show that the V-shaped angles of 1 and 2 are 122.72(15)° and 120.7(4)°, respectively. Intermolecular C-H···O, C-H···N, C-H···π, and π···π interactions link the components into three-dimensional networks in the crystal structures.

Synthesis, growth, structural and optical studies of a new organic three dimensional framework: 4-(aminocarbonyl)pyridine 4-(aminocarbonyl)pyridinium hydrogen L-malate

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

Vijayalakshmi, A.; Vidyavathy, B., E-mail: vidyavathybalraj@gmail.com; Peramaiyan, G.

2017-02-15

4-(aminocarbonyl)pyridine 4-(aminocarbonyl)pyridinium hydrogen L-malate [(4ACP)(4ACP).(LM)] a new organic nonlinear optical (NLO) crystal was grown by the slow evaporation method. Single crystal X-ray diffraction analysis revealed that the [(4ACP)(4ACP).(LM)] crystal belongs to monoclinic crystal system, space group P2{sub 1}/n, with a three dimensional network. Thermogravimetry (TG) and differential thermal (DT) analyses showed that [(4ACP)(4ACP).(LM)] is thermally stable up to 165 °C. The optical transmittance window and the lower cut-off wavelength of [(4ACP)(4ACP).(LM)] were found out by UV–vis–NIR spectral study. The molecular structure of [(4ACP)(4ACP).(LM)] was further confirmed by FTIR spectral studies. The relative dielectric permittivity and dielectric loss were determined asmore » function of frequency and temperature. The third order nonlinear optical property of [(4ACP)(4ACP).(LM)] was studied by the Z-scan technique using a 532 nm diode pumped CW Nd:YAG laser. Nonlinear refractive index, nonlinear absorption coefficient and third order nonlinear susceptibility of the grown crystal were found to be 7.38×10{sup −8} cm{sup 2}/W, 0.08×10{sup −4} cm/W and 5.36×10{sup −6} esu, respectively. The laser damage threshold value is found to be 1.75 GW/cm{sup 2} - Graphical abstract: In the crystal structure of the title complex, the asymmetric unit contains one hydrogen L-malate anion, 4-(aminocarbonyl)pyridinium cation and a neutral isonicotinamide molecule. It is stabilized by intermolecular N-H…O, C-H…O and O-H…O hydrogen bonds which generate a three dimensional network.« less

Ca4As3 – a new binary calcium arsenide

PubMed Central

Hoffmann, Andrea V.; Hlukhyy, Viktor; Fässler, Thomas F.

2015-01-01

The crystal structure of the binary compound tetra­calcium triarsenide, Ca4As3, was investigated by single-crystal X-ray diffraction. Ca4As3 crystallizes in the Ba4P3 structure type and is thus a homologue of isotypic Sr4As3. The unit cell contains 32 Ca2+ cations, 16 As3− isolated anions and four centrosymmetric [As2]4– dumbbells. The As atoms in each of the dumbbells are connected by a single bond, thus this calcium arsenide is a Zintl phase. PMID:26870427

Synthesis, characterization and crystal structure of (2RS,4R)-2-(2-hydroxy-3-methoxyphenyl)thiazolidine-4-carboxylic acid

NASA Astrophysics Data System (ADS)

Muche, Simon; Müller, Matthias; Hołyńska, Małgorzata

2018-03-01

The condensation reaction of ortho-vanillin and L-cysteine leads to formation of a racemic mixture of (2RS,4R)-2-(2-hydroxy-3-methoxyphenyl)thiazolidine-4-carboxylic acid and not, as reported in the available literature, to a Schiff base. The racemic mixture was fully characterized by 1D and 2D NMR techniques, ESI-MS and X-ray diffraction. Addition of ZnCl2 led to formation of crystals in form of colorless needles, suitable for X-ray diffraction studies. The measured crystals were identified as the diastereomer (2R,4R)-2-(2-hydroxy-3-methoxyphenyl)thiazolidine-4-carboxylic acid 1. The bulk material is racemic. Thiazolidine exists as zwitterion in solid state, as indicated by the crystal structure.

Infrared-active optical phonons in LiFePO 4 single crystals

DOE PAGES

Stanislavchuk, T. N.; Middlemiss, D. S.; Syzdek, J. S.; ...

2017-07-28

Infrared-active optical phonons were studied in olivine LiFePO 4 oriented single crystals by means of both rotating analyzer and rotating compensator spectroscopic ellipsometry in the spectral range between 50 and 1400 cm -1. The eigenfrequencies, oscillator strengths, and broadenings of the phonon modes were determined from fits of the anisotropic harmonic oscillator model to the data. Optical phonons in a heterosite FePO 4 crystal were measured from the delithiated ab-surface of the LiFePO 4 crystal and compared with the phonon modes of the latter. Good agreement was found between experimental data and the results of solid-state hybrid density functional theorymore » calculations for the phonon modes in both LiFePO 4 and FePO 4.« less

Thermal Characterization, Crystal Field Analysis and In-Band Pumped Laser Performance of Er Doped NaY(WO4)2 Disordered Laser Crystals

PubMed Central

Serrano, María Dolores; Cascales, Concepción; Han, Xiumei; Zaldo, Carlos; Jezowski, Andrzej; Stachowiak, Piotr; Ter-Gabrielyan, Nikolay; Fromzel, Viktor; Dubinskii, Mark

2013-01-01

Undoped and Er-doped NaY(WO4)2 disordered single crystals have been grown by the Czochralski technique. The specific heat and thermal conductivity (κ) of these crystals have been characterized from T = 4 K to 700 K and 360 K, respectively. It is shown that κ exhibits anisotropy characteristic of single crystals as well as a κ(T) behavior observed in glasses, with a saturation mean free phonon path of 3.6 Å and 4.5 Å for propagation along a and c crystal axes, respectively. The relative energy positions and irreducible representations of Stark Er3+ levels up to 4G7/2 multiplet have been determined by the combination of experimental low (<10 K) temperature optical absorption and photoluminescence measurements and simulations with a single-electron Hamiltonian including both free-ion and crystal field interactions. Absorption, emission and gain cross sections of the 4I13/2↔4I15/2 laser related transition have been determined at 77 K. The 4I13/2 Er3+ lifetime (τ) was measured in the temperature range of 77–300 K, and was found to change from τ (77K) ≈ 4.5 ms to τ (300K) ≈ 3.5 ms. Laser operation is demonstrated at 77 K and 300 K by resonantly pumping the 4I13/2 multiplet at λ≈1500 nm with a broadband (FWHM≈20 nm) diode laser source perfectly matching the 77 K crystal 4I15/2 → 4I13/2 absorption profile. At 77 K as much as 5.5 W of output power were obtained in π-polarized configuration with a slope efficiency versus absorbed pump power of 57%, the free running laser wavelength in air was λ≈1611 nm with the laser output bandwidth of 3.5 nm. The laser emission was tunable over 30.7 nm, from 1590.7 nm to 1621.4 nm, for the same π-polarized configuration. PMID:23555664

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.

Crystallization and preliminary X-ray crystallographic analysis of carboxyl-terminal region 4 of SigR from Streptomyces coelicolor A3(2)

PubMed Central

Kim, Keon Young; Kim, Sunmin; Park, Jeong Kuk; Song, HyoJin; Park, SangYoun

2014-01-01

Full-length SigR from Streptomyces coelicolor A3(2) was overexpressed in Escherichia coli, purified and submitted to crystallization trials using either polyethylene glycol 3350 or 4000 as a precipitant. X-ray diffraction data were collected to 2.60 Å resolution under cryoconditions using synchrotron X-rays. The crystal packs in space group P43212, with unit-cell parameters a = b = 42.14, c = 102.02 Å. According to the Matthews coefficient, the crystal asymmetric unit cannot contain the full-length protein. Molecular replacement with the known structures of region 2 and region 4 as independent search models indicates that the crystal contains only the −35 element-binding carboxyl-terminal region 4 of full-length SigR. Mass-spectrometric analysis of the harvested crystal confirms this, suggesting a crystal volume per protein weight (V M) of 2.24 Å3 Da−1 and 45.1% solvent content. PMID:24915084

Acoustic band gaps of the woodpile sonic crystal with the simple cubic lattice

NASA Astrophysics Data System (ADS)

Wu, Liang-Yu; Chen, Lien-Wen

2011-02-01

This study theoretically and experimentally investigates the acoustic band gap of a three-dimensional woodpile sonic crystal. Such crystals are built by blocks or rods that are orthogonally stacked together. The adjacent layers are perpendicular to each other. The woodpile structure is embedded in air background. Their band structures and transmission spectra are calculated using the finite element method with a periodic boundary condition. The dependence of the band gap on the width of the stacked rods is discussed. The deaf bands in the band structure are observed by comparing with the calculated transmission spectra. The experimental transmission spectra for the Γ-X and Γ-X' directions are also presented. The calculated results are compared with the experimental results.

A Deuterium NMR Study of Bent-Core Liquid Crystals. 1; Synthesis and Characterization of Deuterium-Labeled Oxadiazole-Containing Liquid Crystals

NASA Technical Reports Server (NTRS)

Dingemans, Theo J.; Madsen, Louis A.; Samulski, Edward T.; Bushnell, Dennis M. (Technical Monitor)

2002-01-01

We have synthesized two deuterated boomerang-shaped liquid crystals based on 2,5-bis(4-hydroxyphenyl)-1,3,4-oxadiazole (ODBP). Deuterium was introduced in the rigid 2,5-diphenyl-1,3,4-oxadiazole core and in the aromatic ring of the terminal 4-dodecyloxyphenyl moiety using standard acid catalyzed deuterium exchange conditions. Both compounds, ([4,4'(1,3,4-oxadiazole-2,5-diyl-d4)] di-4-dodecyloxybenzoate: ODBP-d4-Ph-O-C12) and ([4,4'(1,3,4-oxadiazole-2,5-diyl)] di-4-dodecyloxy-benzoate-d4; ODBP-Ph-d4-O-C12) were investigated by nuclear magnetic resonance, optical microscopy and differential scanning calorimetry. The optical textures and thermal behavior of both compounds were found to be identical to the non-deuterated analog [4,4(1,3,4-oxadiazole-2,5-diyl)] di-4-dodecyloxybenzoate (ODBP-Ph-O-C12) which we reported earlier. These compounds exhibit behavior indicative of a biaxial nematic liquid crystal phase, which we hope to confirm using deuterium NMR spectroscopy in the next phase of this study.

Synthesis, growth, structural and optical studies of a new organic three dimensional framework: 4-(aminocarbonyl)pyridine 4-(aminocarbonyl)pyridinium hydrogen L-malate

NASA Astrophysics Data System (ADS)

Vijayalakshmi, A.; Vidyavathy, B.; Peramaiyan, G.; Vinitha, G.

2017-02-01

4-(aminocarbonyl)pyridine 4-(aminocarbonyl)pyridinium hydrogen L-malate [(4ACP)(4ACP).(LM)] a new organic nonlinear optical (NLO) crystal was grown by the slow evaporation method. Single crystal X-ray diffraction analysis revealed that the [(4ACP)(4ACP).(LM)] crystal belongs to monoclinic crystal system, space group P21/n, with a three dimensional network. Thermogravimetry (TG) and differential thermal (DT) analyses showed that [(4ACP)(4ACP).(LM)] is thermally stable up to 165 °C. The optical transmittance window and the lower cut-off wavelength of [(4ACP)(4ACP).(LM)] were found out by UV-vis-NIR spectral study. The molecular structure of [(4ACP)(4ACP).(LM)] was further confirmed by FTIR spectral studies. The relative dielectric permittivity and dielectric loss were determined as function of frequency and temperature. The third order nonlinear optical property of [(4ACP)(4ACP).(LM)] was studied by the Z-scan technique using a 532 nm diode pumped CW Nd:YAG laser. Nonlinear refractive index, nonlinear absorption coefficient and third order nonlinear susceptibility of the grown crystal were found to be 7.38×10-8 cm2/W, 0.08×10-4 cm/W and 5.36×10-6 esu, respectively. The laser damage threshold value is found to be 1.75 GW/cm2

Orthorhombic YBaCo{sub 4}O{sub 8.4} crystals as a result of saturation of hexagonal YBaCo{sub 4}O{sub 7} crystals with oxygen

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

Podberezskaya, N. V., E-mail: podberez@niic.nsc.ru; Bolotina, N. B., E-mail: nb-bolotina@mail.ru; Komarov, V. Yu., E-mail: komarov-v-y@niic.nsc.ru

Hexagonal YBaCo{sub 4}O{sub 7} crystals (sp. gr. P6{sub 3}mc, a{sub h} = 6.3058(4) Å, c{sub h} = 10.2442(7) Å, Z = 2) are saturated with oxygen to the YBaCo{sub 4}O{sub 8.4} composition and studied by X-ray diffraction (XRD) analysis. The saturation is completed by a structural first-order phase transition to orthorhombic crystals (sp. gr. Pbc2{sub 1}, a{sub o} = 31.8419(2) Å, b{sub o} = 10.9239(5) Å, c{sub o} = 10.0960(5) Å, Z = 20). The connection of two lattices is expressed in terms of the action of matrix (500/120/001) on the hexagonal basis. Five structural fragments of the same typemore » but with different degrees of order alternate along the long axis of the oxygen-saturated orthorhombic structure. The XRD data on single crystals differ from the results obtained by other researchers on ceramic samples; possible causes of these differences are discussed.« less

Redox process catalysed by growing crystal-strengite, FePO4,2H2O, crystallizing from solution with iron(II) and hydroxylamine

NASA Astrophysics Data System (ADS)

Lundager Madsen, Hans Erik

2014-09-01

In an attempt to grow pure crystals of the iron(II) phosphate vivianite, Fe3(PO4)2,8H2O, from a solution of Mohr's salt, Fe(NH4)2(SO4)2,6H2O, added to a solution of ammonium phosphate, hydroxylammonium chloride, NH3OHCl, was added to the iron(II) stock solution to eliminate oxidation of iron(II) by oxygen from the air. However, the effect turned out to be the opposite of the expected: whereas hydroxylamine reduces iron(III) in bulk solution, it acted as a strong oxidant in the presence of growing iron phosphate crystals, causing the crystallization of the iron(III) phosphate strengite, FePO4,2H2O, as the only solid phase. Evidently the crystal surface catalyses oxidation of iron(II) by hydroxylamine. The usual composite kinetics of spiral growth and surface nucleation was found. The surface-nucleation part yielded edge free energy λ in the range 12-45 pJ/m, virtually independent of temperature and in the range typical for phosphates of divalent metals. The scatter of values for λ presumably arises from contributions from different crystal forms to the overall growth rate. The low mean value points to strong adsorption of iron(II), which is subsequently oxidized at the crystal surface, forming strengite. The state of the system did not tend to thermodynamic equilibrium, but to a metastable state, presumably controlled by the iron(II) rich surface layer of the crystal. In addition to crystal growth, it was possible to measure nucleation kinetics by light scattering (turbidimetry). A point of transition from heterogeneous to homogeneous nucleation was found, and from the results for the homogeneous domain a rather precise value of crystal surface free energy γ=55 mJ/m2 was found. This is a relatively low value as well, indicating that the redox process plays a role already at the nucleation stage.

Polarized spectral properties and potential application of large-size Nd3+:Ba3Gd2(BO3)4 crystal

NASA Astrophysics Data System (ADS)

Gao, S. F.; Lv, S. Z.; Zhu, Z. J.; Wang, Y.; You, Z. Y.; Li, J. F.; Xu, J. L.; Wang, H. Y.; Tu, C. Y.

2014-06-01

The Nd3+-doped Ba3Gd2(BO3)4 crystal with high optical quality and large size is reported in this paper. The growing processes and characteristics of Nd3+:Ba3Gd2(BO3)4 crystal are discussed. The absorption and luminescence spectra of Nd3+ in Ba3Gd2(BO3)4 crystal were measured at room temperature. The luminescence decay curve in correspondence with the 4F3/2 →4I11/2 transition centered at 1062 nm was also measured. The JO intensity parameters Ωt (t = 2,4,6) were calculated to be Ω2 = 1.263, Ω4 = 2.496, Ω6 = 3.606. The radiative lifetime τr and fluorescence lifetime τf are 317.771 and 115 μs respectively, and the fluorescence quantum efficiency is 37.1%.

Extracting Optical Fiber Background from Surface-Enhanced Raman Spectroscopy Spectra Based on Bi-Objective Optimization Modeling.

PubMed

Huang, Jie; Shi, Tielin; Tang, Zirong; Zhu, Wei; Liao, Guanglan; Li, Xiaoping; Gong, Bo; Zhou, Tengyuan

2017-08-01

We propose a bi-objective optimization model for extracting optical fiber background from the measured surface-enhanced Raman spectroscopy (SERS) spectrum of the target sample in the application of fiber optic SERS. The model is built using curve fitting to resolve the SERS spectrum into several individual bands, and simultaneously matching some resolved bands with the measured background spectrum. The Pearson correlation coefficient is selected as the similarity index and its maximum value is pursued during the spectral matching process. An algorithm is proposed, programmed, and demonstrated successfully in extracting optical fiber background or fluorescence background from the measured SERS spectra of rhodamine 6G (R6G) and crystal violet (CV). The proposed model not only can be applied to remove optical fiber background or fluorescence background for SERS spectra, but also can be transferred to conventional Raman spectra recorded using fiber optic instrumentation.

CFA-4 - a fluorinated metal-organic framework with exchangeable interchannel cations.

PubMed

Fritzsche, J; Grzywa, M; Denysenko, D; Bon, V; Senkovska, I; Kaskel, S; Volkmer, D

2017-05-23

The syntheses and crystal structures of the fluorinated linker 1,4-bis(3,5-bis(trifluoromethyl)-1H-pyrazole-4-yl)benzene (H 2 -tfpb; 1) and the novel metal-organic framework family M[CFA-4] (Coordination Framework Augsburg University-4), M[Cu 5 (tfpb) 3 ] (M = Cu(i), K, Cs, Ca(0.5)), are described. The ligand 1 is fully characterized by single crystal X-ray diffraction, photoluminescence-, NMR-, IR spectroscopy, and mass spectrometry. The copper(i)-containing MOF crystallizes in the hexagonal crystal system within the chiral space group P6 3 22 (no. 182) and the unit cell parameters are as follows: a = 23.630(5) Å, c = 41.390(5) Å, V = 20 015(6) Å 3 . M[CFA-4] features a porous 3-D structure constructed from pentanuclear copper(i) secondary building units {Cu(pz) 6 } - (pz = pyrazolate). Cu(I)[CFA-4] is fully characterized by synchrotron single crystal X-ray diffraction, thermogravimetric analysis, variable temperature powder X-ray diffraction, IR spectroscopy, photoluminescence and gas sorption measurements. Moreover, thermal stability and gas sorption properties of K[CFA-4] and Cu(I)[CFA-4] are compared.

Snynthesis and magnetization of BaLn2O4 (Ln = lanthanide)

NASA Astrophysics Data System (ADS)

Lundberg, Matthew

The BaLn2O4 family has been synthesized successfully as single crystals by the flux-growth method. The phases crystallize in the CaV2O4 structure prototype in space group Pnma (# 62). The structure has been studied using single-crystal x-ray diffraction, and stoichiometry confirmed with EDS, and the unit cell parameters and atomic positions have been determined for the whole lanthanide series (with the exception of the Lu compound). The effects of the lanthanide ionic radius on the atomic positions in the unit cell has been studied in terms of fractional atomic coordinates, bond lengths and angles, and bond valence sums. Magnetic measurements have been performed on the series with the exception of the La, Eu, and Lu members in the form of susceptibility versus temperature. The crystals all show signs of geometric antiferromagnetic frustration with the Neel temperatures significantly below the temperature predicted by the Weiss constant. Additionally some members of the family, namely BaCe2O4, BaNd2O4, BaPr 2O4, BaSm2O4, BaTb2O 4, and BaYb2O4 show significant crystal field splitting, that causes deviation from Currie-Weiss behavior.

Radioactive contamination of scintillators

NASA Astrophysics Data System (ADS)

Danevich, F. A.; Tretyak, V. I.

2018-03-01

Low counting experiments (search for double β decay and dark matter particles, measurements of neutrino fluxes from different sources, search for hypothetical nuclear and subnuclear processes, low background α, β, γ spectrometry) require extremely low background of a detector. Scintillators are widely used to search for rare events both as conventional scintillation detectors and as cryogenic scintillating bolometers. Radioactive contamination of a scintillation material plays a key role to reach low level of background. Origin and nature of radioactive contamination of scintillators, experimental methods and results are reviewed. A programme to develop radiopure crystal scintillators for low counting experiments is discussed briefly.

GEANT4-based full simulation of the PADME experiment at the DAΦNE BTF

NASA Astrophysics Data System (ADS)

Leonardi, E.; Kozhuharov, V.; Raggi, M.; Valente, P.

2017-10-01

A possible solution to the dark matter problem postulates that dark particles can interact with Standard Model particles only through a new force mediated by a “portal”. If the new force has a U(1) gauge structure, the “portal” is a massive photon-like vector particle, called dark photon or A‧. The PADME experiment at the DAΦNE Beam-Test Facility (BTF) in Frascati is designed to detect dark photons produced in positron on fixed target annihilations decaying to dark matter (e+e-→γA‧) by measuring the final state missing mass. The experiment will be composed of a thin active diamond target where a 550 MeV positron beam will impinge to produce e+e- annihilation events. The surviving beam will be deflected with a magnet while the photons produced in the annihilation will be measured by a calorimeter composed of BGO crystals. To reject the background from Bremsstrahlung gamma production, a set of segmented plastic scintillator vetoes will be used to detect positrons exiting the target with an energy lower than that of the beam, while a fast small angle calorimeter will be used to reject the e+e-→γγ(γ) background. To optimize the experimental layout in terms of signal acceptance and background rejection, the full layout of the experiment was modelled with the GEANT4 simulation package. In this paper we will describe the details of the simulation and report on the results obtained with the software.

Imaging birefringent crystals using micro optical coherence tomography (Conference Presentation)

NASA Astrophysics Data System (ADS)

Sharma, Gargi; Singh, Kanwarpal; Gardecki, Joseph A.; Tearney, Guillermo J.

2017-02-01

Background: Uric acid crystals have recently been identified as a possible therapeutic target for coronary artery disease. Being subcellular in size, it is difficult to identify these crystals in situ. Micro optical coherence tomography (Micro-OCT) allows one to image subcellular structures with 1-micron resolution. Even though Micro-OCT should be capable of resolving urate crystals, it's difficult to differentiate these structures from other scattering particles within tissue. In this work we developed a novel polarization sensitive micro OCT (ps-Micro-OCT) system for identification of uric acid crystals. Methods: A spectrometer based ps-Micro-OCT system was developed using a broadband light source. The broadband input light was divided into reference and sample signals using a beam splitter. The reference signal was further divided into two polarized signals with different polarization states. Reflected reference and sample signals were combined and sent to a spectrometer that recorded the interference signal. Results: To test the performance of system, a mirror was used as sample and a quarter wave-plate was placed in the sample path. The measured quarter wave-plate angle values matched closely to actual angle values. Next we prepared uric acid crystals in our lab and imaged them using this system.We were able to image and identify these crystals based on polarization measurements. Conclusion: In this work we imaged and identified uric acid crystals using a newly developed ps-Micro-OCT system. The proposed technique will enable imaging uric acid crystals in coronary artery.

Ca3La2(BO3)4 crystal: a new candidate host material for the ytterbium ion

NASA Astrophysics Data System (ADS)

Wang, Yeqing; You, Zhenyu; Zhu, Zhaojie; Xu, Jinlong; Li, Jianfu; Wang, Yan; Wang, Hongyan; Tu, Chaoyang

2013-10-01

A disordered laser crystal Yb3+-doped Ca3La2(BO3)4 crystal was grown by the Czochralski technique. The characterized room temperature polarized spectra, re-absorption possibility and laser performance showed that this crystal should be a promising gain material, not only suitable for diode pumping, but also a good candidate for the generation of tunable and short pulse lasers. End pumped by a diode laser at 976 nm in plano-concave and plano-plano cavity, a 3.65 W output power with a slope efficiency of 65% was achieved by using a c-cut Yb3+:Ca3La2(BO3)4 crystal. The output laser wavelength shifted from 1042 to 1062 nm.

Crystal structure, electronic structure, optical and scintillation properties of self-activated Cs 4YbI 6 [Crystal structure, optical and scintillation properties of self-activated Cs 4YbI 6

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

Wu, Yuntao; Chakoumakos, Bryan C.; Shi, Hongliang

A self-activated Cs 4YbI 6 single crystal was grown by the vertical Bridgman method. Crystal structure refinements verified the phase purity and the trigonal crystal system with a space group of more » $$\\bar{R}$$3 c. By using differential scanning calorimetry, the melting and crystallization points were determined to be 550 and 510 °C, respectively. Luminescence and scintillation properties were systematically studied. Upon ultraviolet light (360 nm) excitation, the Cs 4YbI 6 crystal exhibits bluish-green emission centered at 450 and 480 nm due to spin-allowed and spin-forbidden transitions of Yb 2+ activators. The lifetimes of the corresponding emission bands at room temperature are tens and hundreds of nanoseconds, respectively. X-ray excited radioluminescence spectrum is dominated by the spin-forbidden transition of Yb 2+ at 480 nm. The absolute light yield is 2700 ± 200 photons/MeV with a principal scintillation decay time of 33 ns. In conclusion, the physical explanation for the low light yield observed is proposed from experimental and theoretical insights.« less

Crystal structure, electronic structure, optical and scintillation properties of self-activated Cs 4YbI 6 [Crystal structure, optical and scintillation properties of self-activated Cs 4YbI 6

DOE PAGES

Wu, Yuntao; Chakoumakos, Bryan C.; Shi, Hongliang; ...

2018-05-14

A self-activated Cs 4YbI 6 single crystal was grown by the vertical Bridgman method. Crystal structure refinements verified the phase purity and the trigonal crystal system with a space group of more » $$\\bar{R}$$3 c. By using differential scanning calorimetry, the melting and crystallization points were determined to be 550 and 510 °C, respectively. Luminescence and scintillation properties were systematically studied. Upon ultraviolet light (360 nm) excitation, the Cs 4YbI 6 crystal exhibits bluish-green emission centered at 450 and 480 nm due to spin-allowed and spin-forbidden transitions of Yb 2+ activators. The lifetimes of the corresponding emission bands at room temperature are tens and hundreds of nanoseconds, respectively. X-ray excited radioluminescence spectrum is dominated by the spin-forbidden transition of Yb 2+ at 480 nm. The absolute light yield is 2700 ± 200 photons/MeV with a principal scintillation decay time of 33 ns. In conclusion, the physical explanation for the low light yield observed is proposed from experimental and theoretical insights.« less

Protein Crystallization Using Room Temperature Ionic Fluids

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Paley, Mark Steve; Turner, Megan B.; Rogers, Robin D.

2006-01-01

The ionic liquids (ILs) 1-butyl-3-methylimidizolium chloride (C4mim-C1), 1-butyl-3- methylimidizolium diethyleneglycol monomethylethersulfate ([C4mim]DEMGS), and 1-butyl-1 -methylpyrollidinium dihydrogenphosphate ([p1,4]dhp) were tested for their effects on the crystallization of the proteins canavalin, beta-lactoglobulin B, xylanase, and glucose isomerase, using a standard high throughput screen. The crystallization experiments were set up with the ILs added to the protein solutions at 0.2 and 0.4 M final concentrations. Crystallization droplets were set up at three proteixprecipitant ratios (1:1, 2:1, and 4:l), which served to progressively dilute the effects of the screen components while increasing the equilibrium protein and IL concentrations. Crystals were obtained for all four proteins at a number of conditions where they were not obtained from the IL-free control experiment. Over half of the protein-IL combinations tested had more successful outcomes than negative, where the IL-free crystallization was better than the corresponding IL-containing outcome, relative to the control. One of the most common causes of a negative outcome was solubilization of the protein by the IL, resulting in a clear drop. In one instance, we were able to use the IL-induced solubilizing to obtain beta-lactoglobulin B crystals from conditions that gave precipitated protein in the absence of IL. The results suggest that it may be feasible to develop ILs specifically for the task of macromolecule crystallization.

Growth and characterization of metal doped and quasi mixed crystals based on ZnCd(SCN)4

NASA Astrophysics Data System (ADS)

Latha, C.; Mahadevan, C. K.; Guo, Li; Liu, Jinghe

2018-03-01

In order to understand the effect of forming hybrid crystals by doping with metallic impurities or by quasi mixing on the physicochemical properties of the basic material crystal, we have grown by the free evaporation method at room temperature and characterized (chemically, structurally, optically and electrically) un-doped and K+/Ca2+/Mn2+/Mg2+/Cu2+ doped (with 1 mol% concentration) ZnCd(SCN)4 and ZnxCd(2-x)(SCN)4 (with x = 0.0, 0.4, 0.8, 1.2, 1.6 and 2.0) single crystals. Single crystals could be grown with x = 0.0 (leading to Cd(SCN)2) but not when x = 2.0 (leading to Zn(SCN)2). Results obtained in the present study through X-ray diffraction and EDAX spectral measurements indicate the formation of the above hybrid crystals. The optical (UV-Vis-NIR spectral and SHG efficiency) measurements indicate significant changes in optical transmittance and SHG efficiency due to doping as well as quasi mixing. Dielectric measurements made in the temperature range 40-150 °C with a fixed frequency of 1 kHz indicate a normal dielectric behavior for all the eleven crystals grown. Moreover, the present study indicates an increase of dielectric constant and SHG efficiency when ZnCd(SCN)4 crystal is doped with a metallic impurity whereas a decrease of dielectric constant and SHG efficiency when quasi mixing is done.

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

NASA Astrophysics Data System (ADS)

Vasenko, Liubov; Qu, Haiyan

2017-02-01

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

Crystallization of the carboxy-terminal region of the bacteriophage T4 proximal long tail fibre protein gp34

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

Granell, Meritxell; Namura, Mikiyoshi; Alvira, Sara

2014-06-19

The crystallization of three C-terminal fragments of the bacteriophage T4 protein gp34 is reported. Diffraction data have been obtained for three native crystal forms and two selenomethionine derivatives, one of which contained high-quality anomalous signal.

Macromolecular Crystallization with Microfluidic Free-Interface Diffusion

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

Segelke, B

2005-02-24

Fluidigm released the Topaz 1.96 and 4.96 crystallization chips in the fall of 2004. Topaz 1.96 and 4.96 are the latest evolution of Fluidigm's microfluidics crystallization technologies that enable ultra low volume rapid screening for macromolecular crystallization. Topaz 1.96 and 4.96 are similar to each other but represent a major redesign of the Topaz system and have of substantially improved ease of automation and ease of use, improved efficiency and even further reduced amount of material needed. With the release of the new Topaz system, Fluidigm continues to set the standard in low volume crystallization screening which is having anmore » increasing impact in the field of structural genomics, and structural biology more generally. In to the future we are likely to see further optimization and increased utility of the Topaz crystallization system, but we are also likely to see further innovation and the emergence of competing technologies.« less

Optical biosensor based on liquid crystal droplets for detection of cholic acid

NASA Astrophysics Data System (ADS)

Niu, Xiaofang; Luo, Dan; Chen, Rui; Wang, Fei; Sun, Xiaowei; Dai, Haitao

2016-12-01

A highly sensitive cholic acid biosensor based on 4-cyano-4‧-penthlbiphenyl (5CB) Liquid crystal droplets in phosphate buffer saline solution was reported. A radial-to-bipolar transition of 5CB droplet would be triggered during competitive reaction of CA at the sodium dodecyl sulfate surfactant-laden 5CB droplet surface. Our liquid crystal droplet sensor is a low-cost, simple and fast method for CA detection. The detection limit (5 μM) of our method is 2.4 times lower than previously report by using liquid crystal film to detection of CA.

The Effect of Pre-irradiation Defects on the Recombination Luminescence in Activated Crystals K2SO4

NASA Astrophysics Data System (ADS)

Koketai, Temirgaly; Tagayeva, Batima; Tussupbekova, Ainura; Mussenova, Elmira

The recombinational luminescence of crystals of K2SO4-Mn2+ and K2SO4-Ni2+ is studied in the article. It is established that impurity ions form the radiation induced centers. The cause of changes of the distribution of lightsum on TSL peaks of a matrix is established. It is proposed that it is related to pre-radiation defeсts in crystals. It is established from this effect that ions of Mn2+ and Ni2+ selectively replace cations in a crystal lattice of potassium sulfate.

Intracellular ice and cell survival in cryo-exposed embryonic axes of recalcitrant seeds of Acer saccharinum: an ultrastructural study of factors affecting cell and ice structures

PubMed Central

Wesley-Smith, James; Berjak, Patricia; Pammenter, N. W.; Walters, Christina

2014-01-01

Background and Aims Cryopreservation is the only long-term conservation strategy available for germplasm of recalcitrant-seeded species. Efforts to cryopreserve this form of germplasm are hampered by potentially lethal intracellular freezing events; thus, it is important to understand the relationships among cryo-exposure techniques, water content, structure and survival. Methods Undried embryonic axes of Acer saccharinum and those rapidly dried to two different water contents were cooled at three rates and re-warmed at two rates. Ultrastructural observations were carried out on radicle and shoot tips prepared by freeze-fracture and freeze-substitution to assess immediate (i.e. pre-thaw) responses to cooling treatments. Survival of axes was assessed in vitro. Key Results Intracellular ice formation was not necessarily lethal. Embryo cells survived when crystal diameter was between 0·2 and 0·4 µm and fewer than 20 crystals were distributed per μm2 in the cytoplasm. Ice was not uniformly distributed within the cells. In fully hydrated axes cooled at an intermediate rate, the interiors of many organelles were apparently ice-free; this may have prevented the disruption of vital intracellular machinery. Intracytoplasmic ice formation did not apparently impact the integrity of the plasmalemma. The maximum number of ice crystals was far greater in shoot apices, which were more sensitive than radicles to cryo-exposure. Conclusions The findings challenge the accepted paradigm that intracellular ice formation is always lethal, as the results show that cells can survive intracellular ice if crystals are small and localized in the cytoplasm. Further understanding of the interactions among water content, cooling rate, cell structure and ice structure is required to optimize cryopreservation treatments without undue reliance on empirical approaches. PMID:24368198

Trithallium hydrogen bis(sulfate), Tl(3)H(SO(4))(2), in the super-ionic phase by X-ray powder diffraction.

PubMed

Matsuo, Yasumitsu; Kawachi, Shinya; Shimizu, Yuya; Ikehata, Seiichiro

2002-07-01

The structure of trithallium hydrogen bis(sulfate), Tl(3)H(SO(4))(2), in the super-ionic phase has been analyzed by Rietveld analysis of the X-ray powder diffraction pattern. Atomic parameters based on the isotypic Rb(3)H(SeO(4))(2) crystal in space group R3m in the super-ionic phase were used as the starting model, because it has been shown from the comparison of thermal and electric properties in Tl(3)H(SO(4))(2) and M(3)H(SO(4))(2) type crystals (M = Rb, Cs or NH(4)) that the room-temperature Tl(3)H(SO(4))(2) phase is isostructural with the high-temperature R3m-symmetry M(3)H(SO(4))(2) crystals. The structure was determined in the trigonal space group R3m and the Rietveld refinement shows that an hydrogen-bond O-H...O separation is slightly shortened compared with O-H...O separations in isotypic M(3)H(SeO(4))(2) crystals. In addition, it was found that the distortion of the SO(4) tetrahedra in Tl(3)H(SO(4))(2) is less than that in isotypic crystals.

Electrical delay line multiplexing for pulsed mode radiation detectors

NASA Astrophysics Data System (ADS)

Vinke, Ruud; Yeom, Jung Yeol; Levin, Craig S.

2015-04-01

Medical imaging systems are composed of a large number of position sensitive radiation detectors to provide high resolution imaging. For example, whole-body Positron Emission Tomography (PET) systems are typically composed of thousands of scintillation crystal elements, which are coupled to photosensors. Thus, PET systems greatly benefit from methods to reduce the number of data acquisition channels, in order to reduce the system development cost and complexity. In this paper we present an electrical delay line multiplexing scheme that can significantly reduce the number of readout channels, while preserving the signal integrity required for good time resolution performance. We experimented with two 4 × 4 LYSO crystal arrays, with crystal elements having 3 mm × 3 mm × 5 mm and 3 mm × 3 mm × 20 mm dimensions, coupled to 16 Hamamatsu MPPC S10931-050P SiPM elements. Results show that each crystal could be accurately identified, even in the presence of scintillation light sharing and inter-crystal Compton scatter among neighboring crystal elements. The multiplexing configuration degraded the coincidence timing resolution from ∼243 ps FWHM to ∼272 ps FWHM when 16 SiPM signals were combined into a single channel for the 4 × 4 LYSO crystal array with 3 mm × 3 mm × 20 mm crystal element dimensions, in coincidence with a 3 mm × 3 mm × 5 mm LYSO crystal pixel. The method is flexible to allow multiplexing configurations across different block detectors, and is scalable to an entire ring of detectors.

New PDLC materials obtained from dispersion of LC under microgravity

NASA Astrophysics Data System (ADS)

Matos, M. R.; Leitao, J. C.; Andre, R. M.; Zambujal, R.; Carmelo Rosa, Carla; Simeao Carvalho, P.; Podgorski, Thomas

Aknowledgements: This project has been supported by ESA-Education, the University of Porto, IFIMUP and INESC-Porto. Bibliography: [1] F Bloisi and L Vicari. Optical Applications of Liquid Crystals, chapter 4: Polymer-dispersed liquid crystals. Institute of Physics Publishing, 2003. [2] J. William Doane. Liquid Crystals Applications and Uses, volume 1, chapter 14: Polymer Dispersed Liquid Crystal Displays, pages 361-391. World Scientific, 1990. [3] K. Parbhakar, J. M. Jin, H. M. Nguyen, and L. H. Dao. Effect of microgravity on the distribution of liquid-crystal droplets dispersed in a polymer matrix. CHEMISTRY OF MA-TERIALS, 8(??):1210-1216, Jun 1996. [4] Paul S. Drzaic. Liquid Crystal Dispersions, volume 1. World Scientific, 1995.

Potassium-cobalt sulphate crystal growth assisted by low frequency vibrations

NASA Astrophysics Data System (ADS)

Sadovsky, A.; Ermochenkov, I.; Dubovenko, E.; Sukhanova, E.; Bebyakin, M.; Dubov, V.; Avetissov, I.

2018-02-01

Single crystals of K2Co(SO4)2·6H2O were grown from solution using the temperature reduction method enhanced by the axial low frequency vibration control technique (AVC-technique). Physical modeling of heat-mass transfer in solution under the AVC action was performed. The growth rate of the AVC grown crystal was found to be twice that of the crystal grown under natural convection conditions. Analysis of spectral characteristics (absorption and Raman spectra) as well as structural properties (dislocation density and microhardness) of the grown crystals showed the significant superiority of the AVC technique for the growth of K2Co(SO4)2·6H2O crystals.

Chalcogen (O2, S, Se, Te) atmosphere annealing induced bulk superconductivity in Fe1+yTe1-xSex single crystal

NASA Astrophysics Data System (ADS)

Sun, Y.; Tsuchiya, Y.; Yamada, T.; Taen, T.; Pyon, S.; Shi, Z. X.; Tamegai, T.

2014-09-01

We reported a detailed study of Fe1+yTe0.6Se0.4 single crystals annealed in the atmosphere of chalcogens (O2, S, Se, Te). After annealing with appropriate amount of chalcogens, Fe1+yTe0.6Se0.4 single crystals show Tc higher than 14 K with a sharp transition width ∼1 K. Critical current density Jc for the annealed crystals reach a very high value ∼2-4 × 105 A/cm2 under zero field, and is also robust under applied field at low temperatures. Magneto-optical imaging reveal that the Jc is homogeneously distributed in the annealed crystals and isotropic in the ab-plane. Our results show that annealing in the atmosphere of chalcogens can successfully induce bulk superconductivity in Fe1+yTe0.6Se0.4.

Structural, thermal and optical properties of KTi(0.92)La(0.08)OPO4 and KTi(0.94)Nd(0.06)OPO4.

PubMed

Sadhasivam, S; Perumal, Rajesh Narayana; Ramasamy, P

2015-10-05

KTi0.92La0.08OPO4 (KTP:La) and KTi0.94Nd0.06OPO4 (KTP:Nd) single crystals are grown using high temperature top seeded flux growth technique. The strain derived from doping is calculated from Williamson-Hall relation. The packing structure and lattice parameter of the grown crystals are analyzed using single crystal X-ray diffraction. The bonding, distortion and change in inter-atomic distances by strain effects of doping are assessed by Raman spectroscopy. Thermal stabilities of grown crystals are evaluated by specific heat capacity measurement. Pronounced high specific heat capacity is recorded as 1.16 J/gK at 498 K for KTP:Nd. Second harmonic generation intensities are measured for KTP:Nd and KTP:La single crystal. Copyright © 2015 Elsevier B.V. All rights reserved.

Magnetic properties and crystallization kinetics of (Fe 100–xNi x) 80Nb 4Si 2B 14 metal amorphous nanocomposites

DOE PAGES

Aronhime, Natan; Zoghlin, Eli; Keylin, Vladimir; ...

2017-09-26

Fe-Ni based metal amorphous nanocomposites (MANCs) are investigated in the pseudo-binary alloys (Fe 100–xNi x) 80Nb 4Si 2B 14. To optimize the soft magnetic properties of the nanocomposites, primary and secondary crystallization kinetics must be understood. As such, primary and secondary crystallization temperatures are determined by differential scanning calorimetry, and activation energies are calculated, along with the resulting crystalline phases. Time-temperature-transformation diagrams for primary and secondary crystallization in (Fe 70Ni 30) 80Nb 4Si 2B 14 are presented. Saturation magnetization and Curie temperature are determined. In conclusion, the shape of magnetization vs. time curves for (Fe 30Ni 70) 80Nb 4Si 2Bmore » 14 at various temperatures suggest that the secondary crystal product often consumes some of the primary crystalline product.« less

Non-covalent interactions in 2-methylimidazolium copper(II) complex (MeImH)2[Cu(pfbz)4]: Synthesis, characterization, single crystal X-ray structure and packing analysis

NASA Astrophysics Data System (ADS)

Sharma, Raj Pal; Saini, Anju; Kumar, Santosh; Kumar, Jitendra; Sathishkumar, Ranganathan; Venugopalan, Paloth

2017-01-01

A new anionic copper(II) complex, (MeImH)2 [Cu(pfbz)4] (1) where, MeImH = 2-methylimidazolium and pfbz = pentafluorobenzoate has been isolated by reacting copper(II) sulfate pentahydrate, pentafluorobenzoic acid and 2-methylimidazole in ethanol: water mixture in 1:2:2 molar ratio. This complex 1 has been characterized by elemental analysis, thermogravimetric analysis, spectroscopic techniques (UV-Vis, FT-IR) and conductance measurements. The complex salt crystallizes in monoclinic crystal system with space group C2/c. Single crystal X-ray structure determination revealed the presence of discrete ions: [Cu(pfbz)4]2- anion and two 2-methylimidazolium cation (C4H7N2)+. The crystal lattice is stabilized by strong hydrogen bonding and F⋯F interactions between cationic-anionic and the anionic-anionic moieties respectively, besides π-π interactions.

Highly Efficient and Simple Route to Synthesize N-(4-Acetylphenyl)-4-chlorobenzenesulfonamide and Its Crystal Structure

NASA Astrophysics Data System (ADS)

Kobkeatthawin, T.; Chantrapromma, S.; Chidan Kumar, C. S.; Fun, H.-K.

2017-12-01

The one-pot synthesis of N-(4-acetylphenyl)-4-chlorobenzenesulfonamide under base conditions is carried out. The present method offers several advantages such as excellent yields, short reaction times and high purity. The chemical structure was elucidated using 1H-NMR, FT-IR and UV-Vis spectroscopy. The crystal structure of the substance was determined by single crystal X-ray structure analysis. The molecule is in a V-shape. The two substituted benzene rings make the dihedral angle of 84.31(9)°. In the crystal packing, the molecules are linked by N-H···O and C-H···O hydrogen bonds into double chains along the b-axis. The crystal is further stabilized by weak C-H···O, C-Cl···π and π···π interactions.

Electrical and thermoluminescence properties of γ-irradiated La2CuO4 crystals

NASA Astrophysics Data System (ADS)

El-Kolaly, M. A.; Abd El-Kader, H. I.; Kassem, M. E.

1994-12-01

Measurements of the electrical properties of unirradiated as well as ?-irradiated La2CuO4 crystals were carried out at different temperatures in the frequency range of 0.1-100 kHz. Thermoluminescence (TL) studies were also performed on such crystals in the temperature range of 300-600K. The conductivity of the unirradiated La2CuO4 crystals were found to obey the power law frequency dependence at each measured temperature below the transition temperature (Tc = 450K). The activation energies for conduction and dielectric relaxation time have been calculated. The TL response and the dc resistance were found to increase with ?-irradiation dose up to 9-10 kGy. The results showed that the ferroelastic domain walls of La2CuO4 crystal as well as its TL traps are sensitive to ?-raditaion. This material can be used in radiation measurements in the range 225 Gy-10 kGy.

Growth and Spectral Assessment of Yb3+-Doped KBaGd(MoO4)3 Crystal: A Candidate for Ultrashort Pulse and Tunable Lasers

PubMed Central

Yu, Yi; Huang, Yisheng; Zhang, Lizhen; Lin, Zhoubin; Wang, Guofu

2013-01-01

In order to explore new more powerful ultrashort pulse laser and tunable laser for diode-pumping, this paper reports the growth and spectral assessment of Yb3+-doped KBaGd(MoO4)3 crystal. An Yb3+:KBaGd(MoO4)3 crystal with dimensions of 50×40×9 mm3 was grown by the TSSG method from the K2Mo2O7 flux. The investigated spectral properties indicated that Yb3+:KBaGd(MoO4)3 crystal exhibits broad absorption and emission bands, except the large emission and gain cross-sections. This feature of the broad absorption and emission bands is not only suitable for the diode pumping, but also for the production of ultrashort pulses and tunability. Therefore, Yb3+:KBaGd(MoO4)3 crystal can be regarded as a candidate for the ultrashort pulse and tunable lasers. PMID:23349892

Growth and spectral assessment of Yb(3+)-doped KBaGd(MoO4)3 crystal: a candidate for ultrashort pulse and tunable lasers.

PubMed

Yu, Yi; Huang, Yisheng; Zhang, Lizhen; Lin, Zhoubin; Wang, Guofu

2013-01-01

In order to explore new more powerful ultrashort pulse laser and tunable laser for diode-pumping, this paper reports the growth and spectral assessment of Yb(3+)-doped KBaGd(MoO(4))(3) crystal. An Yb(3+):KBaGd(MoO(4))(3) crystal with dimensions of 50×40×9 mm(3) was grown by the TSSG method from the K(2)Mo(2)O(7) flux. The investigated spectral properties indicated that Yb(3+):KBaGd(MoO(4))(3) crystal exhibits broad absorption and emission bands, except the large emission and gain cross-sections. This feature of the broad absorption and emission bands is not only suitable for the diode pumping, but also for the production of ultrashort pulses and tunability. Therefore, Yb(3+):KBaGd(MoO(4))(3) crystal can be regarded as a candidate for the ultrashort pulse and tunable lasers.

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

Kuz'mina, L. G., E-mail: kuzmina@igic.ras.ru; Kucherepa, N. S.; Rodnikova, M. N.

The molecular and crystal structures of two p-alkoxybenzylidene)-p'-toluidines C{sub 2}H{sub 5}O-C{sub 6}H{sub 4}-CH=N-C{sub 6}H{sub 4}-CH{sub 3} (1) and C{sub 4}H{sub 9}O-C{sub 6}H{sub 4}-CH=N-C{sub 6}H{sub 4}-CH{sub 3} (2) are determined by X-ray diffraction. Crystals 1 and 2 contain four and two crystallographically independent molecules, respectively. In 1, the geometry of the independent molecules is almost identical. In 2, the independent molecules differ in the conformation of the alkyl chain, which is disordered in one of them. An analysis of the crystal packing of 2 reveals the alternation of spacious layers formed by loosely packed aliphatic fragments of molecules and layers ofmore » closely packed aromatic fragments, which ensures the formation of the mesogenic phase in the course of melting of crystals 2. In crystal 1, loose aliphatic layers are absent.« less

The Crystal and Molecular Structure of an Asymmetric Diacetylene Monomer, 6-(2-methyl-4-nitroanilino)-2,4-hexadiyne-1-ol

NASA Technical Reports Server (NTRS)

Vlasse, Marcus; Paley, Mark S.

1993-01-01

The crystal and molecular structure of an asymmetric diacetylene monomer has been determined from x-ray diffraction data. The crystals, obtained from an acetone/pentane solution, are orthorhombic, Fdd2 with Z = 16 in a unit cell having dimensions of a = 42.815(6) A, b = 22.224(5) A, c = 4.996(l) A. The structure was solved by direct methods and refined by least- squares techniques to an R(sub F) of 6.4% for 988 reflections and 171 variables. The diacetylene chains are disposed in the unit cell in a complex manner in order to satisfy the hydrogen- bonding, crystal packing, and symmetry requirements of the system. The solid state polymerization mechanism is discussed with respect to the geometric disposition of the diacetylene chains. These chains are far apart and incorrectly oriented with respect to each other to permit polymerization in the crystal by means of 1,4-addition, consistent with the Baughman mechanistic model.

UV-LIGA Microfabrication of 220 GHz Sheet Beam Amplifier Gratings with SU-8 Photoresists

DTIC Science & Technology

2010-01-01

4 4 4a Diethyl ether 3d, RT 0 Tetrahydrofuran (THF) 3d, RT 1 2 4 3 3 Py + pyridinium (Pym) HBr crystals 2d, RT 1 2 3 2 Py + Pym HCl crystals 2d, RT 1...1 1 Acetone + Pym HBr crystals 2d, RT 1 0 Pym dichromate in Py 2d, RT 1 2 1 Pym chlorochromate in Py 2d, RT 4 1 2 1a Propylamine (PA) 2d, RT 1 2 3 2

High-quality single crystal growth and magnetic property of Mn4Ta2O9

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

Crystal structure and phase transformations of calcium yttrium orthophosphate, Ca 3Y(PO 4) 3

NASA Astrophysics Data System (ADS)

Fukuda, Koichiro; Iwata, Tomoyuki; Niwa, Takahiro

2006-11-01

Crystal structure and phase transformations of calcium yttrium orthophosphate Ca 3Y(PO 4) 3 were investigated by X-ray powder diffraction, selected-area electron diffraction, transmission electron microscopy and optical microscopy. The high-temperature phase is isostructural with eulytite, cubic (space group I4¯3d) with a=0.983320(5) nm, V=0.950790(8) nm 3, Z=4 and D x=3.45 Mg m -3. The crystal structure was refined with a split-atom model, in which the oxygen atoms are distributed over two partially occupied sites. Below the stable temperature range of eulytite, the crystal underwent a martensitic transformation, which is accompanied by the formation of platelike surface reliefs. The inverted crystal is triclinic (space group P1) with a=1.5726(1) nm, b=0.84267(9) nm, c=0.81244(8) nm, α=109.739(4)°, β=90.119(5)°, γ=89.908(7)°, V=1.0134(1) nm 3, Z=4 and D x=3.24 Mg m -3. The crystal grains were composed of pseudo-merohedral twins. The adjacent twin domains were related by the pseudo-symmetry mirror planes parallel to {101¯} with the composition surface {101¯}. When the eulytite was cooled relatively slowly from the stable temperature range, the decomposition reaction of Ca 3Y(PO 4) 3→ β-Ca 3(PO 4) 2+YPO 4 occurred.

Multicomponent hydrogen-bonding organic solids constructed from 6-hydroxy-2-naphthoic acid and N-heterocycles: Synthesis, structural characterization and synthon discussion

NASA Astrophysics Data System (ADS)

Zong, Yingxia; Shao, Hui; Pang, Yanyan; Wang, Debao; Liu, Kang; Wang, Lei

2016-07-01

Seven novel multicomponent crystals involving various substituted organic amine molecules and 6-hydroxy-2-naphthoic acid were prepared and characterized by using single crystal X-ray diffraction, infrared and thermogravimetric analyses (TGA). Crystal structures with 1,4-bis(imidazol) butane (L1) 1, 1,4-bis(imidazol-1-ylmethyl)benzene (L2) 2, 1-phenyl piperazine 3, 2-amino-4-hydroxy-6-methyl pyrimidine 4, 4,4'-bipyridine 5, 5,5'-dimethyl-2,2'-dipyridine 6, 2-amino-4,6-dimethyl pyrimidine 7 were determined. Among the seven molecular complexes, total proton transfer from 6-hydroxy-2-naphthoic acid to coformer has occurred in crystals 1-4, while the remaining were cocrystals. X-ray single-crystal structures of these complexes reveal that strong hydrogen bonding O-H···O/N-H···O/O-H···N and weak C-H···O/C-H···π/π···π intermolecular interactions direct the packing modes of molecular crystals together. The analysis of supramolecular synthons in the present structures shows that some classical supramolecular synthons like pyridine-carboxylic acid heterosynthon R22 (7) and aminopyridine-carboxylic acid heterosynthon R22 (8), are again observed in constructing the hydrogen-bonding networks in this paper. Besides, we noticed that water molecules act as a significant hydrogen-bonding connector in constructing supramolecular architectures of 3, 4, 6, and 7.

Influence of crystal characteristics on the shock sensitivities of cyclotrimethylene trinitramine, cyclotetramethylene tetranitramine, and 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetra-cyclo[5,5,0,03,1105,9]dodecane immersed in liquid

NASA Astrophysics Data System (ADS)

Li, Hongzhen; Xu, Rong; Kang, Bing; Li, Jinshan; Zhou, Xiaoqing; Zhang, Chaoyang; Nie, Fude

2013-05-01

The shock sensitivities of differently qualified cyclotrimethylene trinitramine (RDX), cyclotetramethylene tetranitramine(HMX), and 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetra-cyclo[5,5,0,03,1105,9]dodecane (CL-20) immersed in liquid were determined by the large-scale gap tests, for systemic discussion on the influences of crystal characteristics on them. As a result, it shows that (1) the immersion of crystals in liquid leads to an obvious sensitivity decrease; (2) for all three explosives, their shock sensitivities are lowered with increasing their crystal apparent densities or decreasing their particle sizes, and almost not affected by particle morphologies; (3) the crystal twins are readily formed for HMX and the most distinct factor influencing its shock sensitivities; (4) it is found that the crystal apparent density affects most obviously the shock sensitivities for RDX and CL-20; and (5) CL-20, HMX, and RDX are less and less sensitive to shock, suggesting chemical components are also a determining factor.

Low carrier semiconductor like behavior in Lu3Ir4Ge13 single crystal

NASA Astrophysics Data System (ADS)

Kumar, Anil; Matteppanavar, Shidaling; Thamizhavel, A.; Ramakrishnan, S.

2018-04-01

Single crystal of Lu3Ir4Ge13 crystallizing in the Yb3Rh4Sn13-type cubic crystal structure has been grown by Czochralski method in a tetra-arc furnace. In this paper we report on the crystal structure, magnetic and transport properties of Lu3Ir4Ge13. The analysis of the powder x-ray diffraction (XRD) studies revealed that Lu3Ir4Ge13 crystallizes in a cubic structure with the space group Pm-3n, no. 223. The lattice parameter was obtained from the Rietveld refinement of the room temperature XRD data which amounts to 8.904 (3) Å with low R factors. The temperature dependence of the resistivity exhibited semiconductor like behavior till 1.8 K, with a broad hump around 15 - 62 K. This hump was observed in both warming and cooling cycle with a very small hysteresis, it may be due to the existence of structural transition from high - low symmetry. The temperature dependent magnetization data shows the diamagnetic behavior with an anomaly around 70 K, which is well supported by the derivative of resistivity data.

Crystal structure of minoxidil at low temperature and polymorph prediction.

PubMed

Martín-Islán, Africa P; Martín-Ramos, Daniel; Sainz-Díaz, C Ignacio

2008-02-01

An experimental and theoretical investigation on crystal forms of the popular and ubiquitous pharmaceutical Minoxidil is presented here. A new crystallization method is presented for Minoxidil (6-(1-piperidinyl)-2,4-pyrimidinediamide 3-oxide) in ethanol-poly(ethylene glycol), yielding crystals with good quality. The crystal structure is determined at low temperature, with a final R value of 0.035, corresponding to space group P2(1) (monoclinic) with cell dimensions a = 9.357(1) A, b = 8.231(1) A, c = 12.931(2) A, and beta = 90.353(4) degrees . Theoretical calculations of the molecular structure of Minoxidil are set forward using empirical force fields and quantum-mechanical methods. A theoretical prediction for Minoxidil crystal structure shows many possible polymorphs. The predicted crystal structures are compared with X-ray experimental data obtained in our laboratory, and the experimental crystal form is found to be one of the lowest energy polymorphs.

Sodium Chloride Crystal-Induced SERS Platform for Controlled Highly Sensitive Detection of Illicit Drugs.

PubMed

Yu, Borong; Li, Pan; Zhou, Binbin; Tang, Xianghu; Li, Shaofei; Yang, Liangbao

2018-04-03

A sodium chloride crystal-driven spontaneous 'hot spot' structure was demonstrated as a SERS-active platform, to get reproducible SERS signals, and eliminate the need for mapping large areas, in comparison with solution phase testing. During the process of solvent evaporation, the crystals produced induced silver aggregates to assemble around themselves. The micro-scale crystals can also act as a template to obtain an optical position, such that the assembled hot area is conveniently located during SERS measurements. More importantly, the chloride ions added in colloids can also replace the citrate and on the surface of the silver sol, and further decrease the background interference. High quality SERS spectra from heroin, methamphetamine (MAMP), and cocaine have been obtained on the crystal-driven hot spot structure with high sensitivity and credible reproducibility. This approach can not only bring the nanoparticles to form plasmonic hot spots in a controlled way, and thus provide high sensitivity, but also potentially be explored as an active substrate for label-free detection of other illicit drugs or additives. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Synthesis, crystal structure, DFT studies, acid dissociation constant, and antimicrobial activity of methyl 2-(4-chlorophenyl)-7a-((4-chlorophenyl)carbamothioyl)-1-oxo-5,5-diphenyl-3-thioxo-hexahydro-1H-pyrrolo[1,2-e]imidazole-6-carboxylate

NASA Astrophysics Data System (ADS)

Nural, Yahya; Gemili, Muge; Seferoglu, Nurgul; Sahin, Ertan; Ulger, Mahmut; Sari, Hayati

2018-05-01

A novel bicyclic thiohydantoin fused to pyrrolidine compound, methyl 2-(4-chlorophenyl)-7a-((4-chlorophenyl)carbamothioyl)-1-oxo-5,5-diphenyl-3-thioxo-hexahydro-1H-pyrrolo[1,2-e]imidazole-6-carboxylate, was synthesized by the cyclization reaction of dimethyl 5,5-diphenylpyrrolidine-2,4-dicarboxylate and 4-chlorophenyl isothiocyanate in the presence of 4-(dimethylamino)pyridine to form methyl 2-(4-chlorophenyl)-1-oxo-5,5-diphenyl-3-thioxo-hexahydro-1H-pyrrolo[1,2-e]imidazole-6-carboxylate with concomitant addition reaction of the 4-chlorophenyl isothiocyanate in 79% yield. The structural characterization was performed by NMR, FT-IR, MS and HRMS techniques, and the stereochemistry of the compound was determined by single crystal X-ray diffraction study. In addition, the molecular structure and 1H and 13C NMR chemical shifts of the compound were obtained with the density functional theory and Hartree-Fock calculations. Acid dissociation constants of the compound were determined using potentiometric titration method in 25% (v/v) dimethyl sulfoxide-water hydroorganic solvent at 25 ± 0.1 °C, at an ionic background of 0.1 mol/L of NaCl using the HYPERQUAD computer program. Four acid dissociation constants were obtained for the compound, and we suggest that these acid dissociation constants are related to the NH, for two groups of enthiols and enol groups. Antimicrobial activity study was performed against S. aureus, B. subtilis, A. hydrophila, E. coli and A. baumannii as bacterial standard strains, and against M. tuberculosis H37Rv as mycobacterial strain. The compound exhibited antibacterial activity in the range of 31.25-62.5 μg/mL, and antimycobacterial activity with a MIC value of 40 μg/mL against the indicated strains.

Infrared study of OH(-) defects in KTiOPO4 crystals

NASA Astrophysics Data System (ADS)

Morris, P. A.; Crawford, M. K.; Jones, B.

1992-12-01

Variations in the concentrations and distributions of the OH(-) defects present in flux and hydrothermal KTiOPO4 (KTP) crystals, measured by infrared spectroscopy of single crystals, are attributed to differences in the growth environments and other nonhydrogenic defects present in the crystals. The concentrations of OH(-) have been estimated from the infrared data to be approximately 400 ppma (parts per million atomic) (3.0 x 10 exp 19/cu cm) in the flux crystals, 1100-1500 ppma (0.74-1.1 x 10 exp 20/cu cm) in the high-temperature hydrothermal and 600 ppma (4.3 x 10 exp 19/cu cm) in the low-temperature hydrothermal crystals. A 3566/cm peak and a 3575/cm band are observed in all crystals. The integrated intensity of the OH(-) absorption band at 3566/cm increases at the expense of the 3575/cm band at higher temperatures in the high-temperature hydrothermal crystals. Several OH(-) peaks (3490, 3455, 3428, 3420, and 3333/cm), which have strongly temperature-dependent linewidths, are present in the hydrothermally grown KTP crystals. The temperature dependencies of their peak frequencies and widths are consistent with the presence of mobile protons in the lattice. The protons located in the 3490 and 3428/cm sites are believed to contribute to the ionic conductivity of the high-conductivity high-temperature hydrothermal crystals.

Growth of 4-(dimethylamino) benzaldehyde doped triglycine sulphate single crystals and its characterization

NASA Astrophysics Data System (ADS)

Rai, Chitharanjan; Sreenivas, K.; Dharmaprakash, S. M.

2009-11-01

Single crystals of triglycine sulphate (TGS) doped with 1 mol% of 4-(dimethylamino) benzaldehyde (DB) have been grown from aqueous solution at ambient temperature by slow evaporation technique. The effect of dopant on the crystal growth and dielectric, pyroelectric and mechanical properties of TGS crystal have been investigated. X-ray powder diffraction pattern for pure and doped TGS was collected to determine the lattice parameters. FTIR spectra were employed to confirm the presence of 4-(dimethylamino) benzaldehyde in TGS crystal, qualitatively. The dielectric permittivity has been studied as a function of temperature by cooling the sample at a rate of 1 °C/min. An increase in the Curie temperature Tc=51 °C (for pure TGS, Tc=48.5 °C) and decrease in maximum permittivity has been observed for doped TGS when compared to pure TGS crystal. Pyroelectric studies on doped TGS were carried out to determine pyroelectric coefficient. The Vickers's hardness of the doped TGS crystals along (0 1 0) face is higher than that of pure TGS crystal for the same face. Domain patterns on b-cut plates were observed using scanning electron microscope. The low dielectric constant, higher pyroelectric coefficient and higher value of hardness suggest that doped TGS crystals could be a potential material for IR detectors.

Fluorescent Approaches to High Throughput Crystallography

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Forsythe, Elizabeth

2005-01-01

X-ray crystallography remains the primary method for determining the structure of macromolecules. The first requirement is to have crystals, and obtaining them is often the rate-limiting step. The numbers of crystallization trials that are set up for any one protein for structural genomics, and the rate at which they are being set up, now overwhelm the ability for strictly human analysis of the results. Automated analysis methods are now being implemented with varying degrees of success, but these typically cannot reliably extract intermediate results. By covalently modifying a subpopulation, 51%, of a macromolecule solution with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of purification. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination the crystals show up as bright objects against a dark background. As crystalline packing is more dense than amorphous precipitate, the fluorescence intensity can be used as a guide in distinguishing different types of precipitated phases, even in the absence of obvious crystalline features, widening the available potential lead conditions in the absence of clear hits. Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Also, brightly fluorescent crystals are readily found against less fluorescent precipitated phases, which under white light illumination may serve to obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries and by having the protein or protein structures all that show up. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons. This presentation will focus on the methodology for fluorescent labeling, the crystallization results, and the effects of the trace labeling on the crystal quality.

Fluorescent Approaches to High Throughput Crystallography

NASA Technical Reports Server (NTRS)

Minamitani, Elizabeth Forsythe; Pusey, Marc L.

2004-01-01

X-ray crystallography remains the primary method for determining the structure of macromolecules. The first requirement is to have crystals, and obtaining them is often the rate-limiting step. The numbers of crystallization trials that are set up for any one protein for structural genomics, and the rate at which they are being set up, now overwhelm the ability for strictly human analysis of the results. Automated analysis methods are now being implemented with varying degrees of success, but these typically cannot reliably extract intermediate results. By covalently modifying a subpopulation, less than or = 1%, of a macromolecule solution with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of a macromolecules purification. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination the crystals will show up as bright objects against a dark background. As crystalline packing is more dense than amorphous precipitate, the fluorescence intensity can be used as a guide in distinguishing different types of precipitated phases, even in the absence of obvious crystalline features, widening the available potential lead conditions in the absence of clear "bits." Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Also, brightly fluorescent crystals are readily found against less fluorescent precipitated phases, which under white light illumination may serve to obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries and by having the protein or protein structures all that show up. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons. This presentation will focus on the methodology for fluorescent labeling, the crystallization results, and the effects of the trace labeling on the crystal quality.

Fluorescent Approaches to High Throughput Crystallography

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Forsythe, Elizabeth

2004-01-01

X-ray crystallography remains the primary method for determining the structure of macromolecules. The first requirement is to have crystals, and obtaining them is often the rate-limiting step. The numbers of crystallization trials that are set up for any one protein for structural genomics, and the rate at which they are being set up, now overwhelm the ability for strictly human analysis of the results. Automated analysis methods are now being implemented with varying degrees of success, but these typically can not reliably extract intermediate results. By covalently modifying a subpopulation, less than or = 1%, of a macromolecule solution with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of purification. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination the crystals show up as bright objects against a dark background. As crystalline packing is more dense than amorphous precipitate, the fluorescence intensity can be used as a guide in distinguishing different types of precipitated phases, even in the absence of obvious crystalline features, widening the available potential lead conditions in the absence of clear "hits." Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Also, brightly fluorescent crystals are readily found against less fluorescent precipitated phases, which under white light illumination may serve to obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries and by having the protein or protein structures all that show up. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons. This presentation will focus on the methodology for fluorescent labeling, the crystallization results, and the effects of the trace labeling on the crystal quality.

(PCG) Protein Crystal Growth HIV Reverse Transcriptase

NASA Technical Reports Server (NTRS)

1992-01-01

HIV Reverse Transcriptase crystals grown during the USML-1 (STS-50) mission using Commercial Refrigerator/Incubator Module (CR/IM) at 4 degrees C and the Vapor Diffusion Apparatus (VDA). Reverse transcriptase is an enzyme responsible for copying the nucleic acid genome of the AIDS virus from RNA to DNA. Studies indicated that the space-grown crystals were larger and better ordered (beyond 4 angstroms) than were comparable Earth-grown crystals. Principal Investigators were Charles Bugg and Larry DeLucas.

Crystal growth, characterization and theoretical studies of 4-aminopyridinium picrate

NASA Astrophysics Data System (ADS)

Aditya Prasad, A.; Muthu, K.; Rajasekar, M.; Meenatchi, V.; Meenakshisundaram, S. P.

2015-01-01

Single crystals of 4-aminopyridinium picrate (APP) were grown by slow evaporation of a mixed solvent system methanol-acetone (1:1, v/v) containing equimolar quantities of 4-aminopyridine and picric acid. Structure is elucidated by single crystal XRD analysis and the crystal belongs to monoclinic system with four molecules in the unit cell (space group P21/c) and the cell parameter values are, a = 8.513 Å (±0.015), b = 11.33 Å (±0.02), c = 14.33 Å (±0.03) and β = 104.15° (±0.019), V = 1340 A3 (±6) with refined R factors R1 = 0.0053 and wR2 = 0.0126. The electron density mapping is interpreted to find coordinates for each atom in the crystallized molecules. The various functional groups present in the molecule are confirmed by FT-IR analysis. UV-visible spectral analysis was used to determine the band gap energy of 4-aminopyridinium picrate. Powder X-ray diffraction pattern reveals the crystallinity of the as-grown crystal and it closely resembles the simulated XRD from the single crystal XRD analysis. Scanning electron microscopy reveals the surface morphology of the grown crystal. Optimized geometry is derived by Hartree-Fock theory calculations and the first-order molecular hyperpolarizability (β), theoretically calculated bond length, bond angles and excited state energy from theoretical UV-vis spectrum were estimated.

Overexpression, crystallization and preliminary X-ray crystallographic analysis of erythronate-4-phosphate dehydrogenase from Pseudomonas aeruginosa.

PubMed

Ha, Jun Yong; Lee, Ji Hyun; Kim, Kyoung Hoon; Kim, Do Jin; Lee, Hyung Ho; Kim, Hye-Kyung; Yoon, Hye-Jin; Suh, Se Won

2006-02-01

The enzyme erythronate-4-phosphate dehydrogenase catalyses the conversion of erythronate-4-phosphate to 3-hydroxy-4-phospho-hydroxy-alpha-ketobutyrate. It belongs to the D-isomer-specific 2-hydroxyacid dehydrogenase family. It is essential for de novo biosynthesis of vitamin B6 (pyridoxine). Erythronate-4-phosphate dehydrogenase from Pseudomonas aeruginosa, a homodimeric enzyme consisting of two identical 380-residue subunits, has been overexpressed in Escherichia coli with a C-terminal purification tag and crystallized at 297 K using 0.7 M ammonium dihydrogen phosphate, 0.4 M ammonium tartrate, 0.1 M sodium citrate pH 5.6 and 10 mM cupric chloride. X-ray diffraction data were collected to 2.20 A from a crystal grown in the presence of NADH. The crystals belong to the orthorhombic space group P2(1)2(1)2(1), with unit-cell parameters a = 84.77, b = 101.28, c = 142.58 A. A dimeric molecule is present in the asymmetric unit, giving a crystal volume per protein weight (VM) of 3.64 A3 Da(-1) and a solvent content of 66%.

Studies on the growth, structural, spectral and third-order nonlinear optical properties of ammonium 3-carboxy-4-hydroxy benzenesulfonate monohydrate single crystal.

PubMed

Silambarasan, A; Krishna Kumar, M; Thirunavukkarasu, A; Mohan Kumar, R; Umarani, P R

2015-01-25

An organic nonlinear optical bulk single crystal, Ammonium 3-carboxy-4-hydroxy benzenesulfonate monohydrate (ACHBS) was successfully grown by solution growth technique. Single crystal X-ray diffraction study confirms that, the grown crystal belongs to P21/c space group. Powder X-ray diffraction and high resolution X-ray diffraction analyses revealed the crystallinity of the grown crystal. Infrared spectral analysis showed the vibrational behavior of chemical bonds and its functional groups. The thermal stability and decomposition stages of the grown crystal were studied by TG-DTA analysis. UV-Visible transmittance studies showed the transparency region and cut-off wavelength of the grown crystal. The third-order nonlinear optical susceptibility of the grown crystal was estimated by Z-scan technique using He-Ne laser source. The mechanical property of the grown crystal was studied by using Vicker's microhardness test. Copyright © 2014 Elsevier B.V. All rights reserved.

A view inside the nature of protein crystals

NASA Astrophysics Data System (ADS)

Oswald, R.; Pietzsch, M.; Ulrich, J.

2017-07-01

In this work a fundamental analysis of protein crystal modifications was presented to compare and confirm the components of protein crystal modifications. The result is that a protein crystal contains besides the protein, the precipitant and water. A mass spectrometer coupled to a thermogravimetry device was used to confirm the different waters (free water -the chosen buffer- and bound water) inside the crystals. Here the biggest amount of water is the free water (the buffer) with an amount of approximately 35%. The bound water (in the sense of a hydrate) has only an amount of about 1-1.5%. Furthermore, an x-ray analysis to confirm the influence range of pH value on the stability of one crystal modification for the understanding of effects on dissolution mechanism of protein crystals was investigated. The crystals of the tetragonal modification crystallized at pH 4.7, 4.85, 5.0, 5.15 and 5.3 maintain according to the x-ray measurements the same lattice parameters. The measured data are discussed.

Tunable two-dimensional photonic crystals using liquid crystal infiltration

NASA Astrophysics Data System (ADS)

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

2000-01-01

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

Transfiguring structural, optical and dielectric properties of cadmium thiourea acetate crystal by the addition of L-threonine for laser assisted device applications

NASA Astrophysics Data System (ADS)

Kulkarni, Rupali B.; Anis, Mohd; Hussaini, S. S.; Shirsat, Mahendra D.

2018-03-01

Present investigation reports the growth of pure and L-threonine (LT) doped cadmium thiourea acetate (CTA) crystals by slow solution evaporation technique followed by structural, optical and dielectric characterization studies. A bulk single crystal of LT-CTA has been grown at temperature 38 °C. The single crystal x-ray diffraction technique has been employed to confirm the structural parameters of pure and LT doped CTA crystals. The increase in optical transparency of LT-CTA crystal was ascertained in the range of 200 to 900 nm using UV-visible spectral analysis. The widened optical band gap of the LT-CTA crystal is found to be 4.7 eV. Pure and doped crystals are subjected to FT-IR analysis to indicate the presence of functional groups quantitatively. Appreciable enhancement in second harmonic generation (SHG) efficiency of LT-CTA crystal with reference to parent CTA was confirmed from Kurtz-Perry SHG test (1.31 times of CTA crystal). The assertive influence of LT on electrical properties of grown crystals has been investigated in the temperature range 35 °C-120 °C. Electronic purity and the color centered photoluminescence emission nature of pure and IA-CTA crystals were justified by luminescence analysis. With the aid of single beam Z-scan analysis, the Kerr lensing nonlinearity was identified and the magnitude of TONLO parameters has been determined. The cubic susceptibility (χ3) and figure of merit (FOM) was found to be 4.81 × 10-4esu and 978.35. Results vitalize LT-CTA for laser stabilization systems.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Single crystals of (FeIn{sub 2}S{sub 4}){sub x} · (CuIn{sub 5}S{sub 8}){sub 1–x} alloys: Crystal structure, nuclear gamma resonance spectra, and thermal expansion

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

Bodnar, I. V., E-mail: chemzav@bsuir.by; Zhafar, M. A.; Kasyuk, Yu. V.

FeIn{sub 2}S{sub 4} and CuIn{sub 5}S{sub 8} compounds and (FeIn{sub 2}S{sub 4}){sub x} · (CuIn{sub 5}S{sub 8}){sub 1–x} alloy single crystals are grown by planar crystallization. It is shown that both of the initial FeIn{sub 2}S{sub 4} and CuIn{sub 5}S{sub 8} compounds and alloys on their basis crystallize with the formation of the cubic spinel structure. It is established that the unit-cell parameter a linearly varies with the composition parameter x. By means of nuclear gamma resonance spectroscopy in the transmission mode of measurements, the local states of iron ions in the alloys are studied. For the single crystals grownmore » in the study, thermal expansion is explored using the dilatometry technique, the thermal-expansion coefficients are determined, and the Debye temperature and rms (root-mean-square) dynamic displacements are calculated.« less

Crystal Nucleation Using Surface-Energy-Modified Glass Substrates.

PubMed

Nordquist, Kyle A; Schaab, Kevin M; Sha, Jierui; Bond, Andrew H

2017-08-02

Systematic surface energy modifications to glass substrates can induce nucleation and improve crystallization outcomes for small molecule active pharmaceutical ingredients (APIs) and proteins. A comparatively broad probe for function is presented in which various APIs, proteins, organic solvents, aqueous media, surface energy motifs, crystallization methods, form factors, and flat and convex surface energy modifications were examined. Replicate studies ( n ≥ 6) have demonstrated an average reduction in crystallization onset times of 52(4)% (alternatively 52 ± 4%) for acetylsalicylic acid from 91% isopropyl alcohol using two very different techniques: bulk cooling to 0 °C using flat surface energy modifications or microdomain cooling to 4 °C from the interior of a glass capillary having convex surface energy modifications that were immersed in the solution. For thaumatin and bovine pancreatic trypsin, a 32(2)% reduction in crystallization onset times was demonstrated in vapor diffusion experiments ( n ≥ 15). Nucleation site arrays have been engineered onto form factors frequently used in crystallization screening, including microscope slides, vials, and 96- and 384-well high-throughput screening plates. Nucleation using surface energy modifications on the vessels that contain the solutes to be crystallized adds a layer of useful variables to crystallization studies without requiring significant changes to workflows or instrumentation.

Production and relevance of cosmogenic radionuclides in NaI(Tl) crystals

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

Amaré, J.; Cebrián, S.; Cuesta, C.

2015-08-17

The cosmogenic production of long-lived radioactive isotopes in materials is an hazard for experiments demanding ultra-low background conditions. Although NaI(Tl) scintillators have been used in this context for a long time, very few activation data were available. We present results from two 12.5 kg NaI(Tl) detectors, developed within the ANAIS project and installed at the Canfranc Underground Laboratory. The prompt data taking starting made possible a reliable quantification of production of some I, Te and Na isotopes with half-lives larger than ten days. Tnitial activities underground were measured and then production rates at sea level were estimated following the history ofmore » detectors; a comparison of these rates with calculations using typical cosmic neutron flux at sea level and a selected description of excitation functions was also carried out. After including the contribution from the identified cosmogenic products in the detector background model, we found that the presence of {sup 3}H in the crystal bulk would help to fit much better our background model and experimental data. We have analyzed the cosmogenic production of {sup 3}H in NaI, and although precise quantification has not been attempted, we can conclude that it could imply a very relevant contribution to the total background below 15 ke in NaI detectors.« less

Hydrothermal synthesis, crystal structure and properties of 2-D and 3-D lanthanide sulfates

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

Xu Yan; Ding Shaohua; Zheng Xuefang

2007-07-15

Two new lanthanum sulfates DySO{sub 4}(OH) 1 and Eu{sub 2}(SO{sub 4}){sub 3}(H{sub 2}O){sub 8} 2 have been hydrothermally synthesized. The colorless crystals were characterized by IR, TGA, ICP and XRD. The structure was determined by single-crystal X-ray diffraction. 1 crystallizes with monoclinic symmetry, space group P2(1)/n [a=7.995(4) A, b=10.945(5) A, c=8.164(4) A, {alpha}=90{sup o}, {beta}=93.619(6){sup o}, {gamma}=90{sup o}, V=713.0(5) A{sup 3}, Z=8]. It displays a three-dimensional framework, based on the novel Dy-O chains connected by the sulfate groups through helical chains. 2 crystallizes with monoclinic symmetry, space group C2/c, [a=13.5605(17) A, b=6.7676(8) A, c=18.318(2) A, {alpha}=90{sup o}, {beta}=102.265(2){sup o}, {gamma}=90{supmore » o}, V=1642.7 (4) A{sup 3}, Z=4]. Its layered framework is attained by the europium atoms connected by the sulfate groups arranged in a helical manner. - Graphical abstract: Two new lanthanum sulfates DySO{sub 4}(OH) 1 and Eu{sub 2} (SO{sub 4}){sub 3} (H{sub 2}O){sub 8} 2 have been hydrothermally synthesized. The colorless crystals were characterized by IR, TGA, ICP and XRD. The structure was determined by single-crystal X-ray diffraction. It displays a three dimensional framework, based on the novel Dy-O chains connected by the sulfate groups through helical chains.« less

Synthesis, crystal structure, and luminescence properties of a new nitride polymorph, β-Sr0.98Eu0.02AlSi4N7

NASA Astrophysics Data System (ADS)

Yoshimura, Fumitaka; Yamane, Hisanori; Nagasako, Makoto

2018-02-01

Prismatic vermilion single crystals 200 μm-2 mm in size, together with a white powder, were obtained by heating a mixture of binary nitrides containing Mg3N2 at 2030 °C under 0.85 MPa of N2. Yellow, thick-platelet single crystals with sizes of 150-500 μm were also found to grow at or near the surface of the product. Single crystal X-ray diffraction demonstrated that the vermilion crystals were orthorhombic Sr0.98Eu0.02AlSi4N7, which has been prepared in previous studies and is termed the α phase of this compound. The yellow crystals were revealed to be a new polymorph of Sr0.98Eu0.02AlSi4N7 (β phase) that crystalized in a monoclinic cell (a = 8.1062(1) Å, b = 9.0953(1) Å, c = 8.9802(2) Å, β = 111.6550(5)°, space group P21) with twins that could be examined by transmission and scanning transmission electron microscopy. β-Sr0.98Eu0.02AlSi4N7 was found to have a three-dimensional network structure formed by the stacking of two types of layers. One is a dreier layer of (Al/Si)N4 tetrahedra that consists of N vertex-sharing double chains of (Al/Si)N4 tetrahedra extending in the c-axis direction with Sr and Eu atoms aligned between the chains, while the other is a layer of (Al/Si)N4 tetrahedra connected by sharing N edges and vertexes. The crystal structure of β-Sr0.98Eu0.02AlSi4N7 is similar to those of certain oxynitrides, such as Sr3Al3+xSi13-xN21-xO2+x:Eu2+ (x ≈ 0) and Sr4.9Eu0.1Al5+xSi21-xN35-xO2+x (x ≈ 0). The peak wavelength and full width at half maximum in the emission spectrum obtained from single crystals of β-Sr0.98Eu0.02AlSi4N7 under excitation at 400 nm were 541 and 66 nm, respectively.

Patterns of calcium oxalate monohydrate crystallization in complex biological systems

NASA Astrophysics Data System (ADS)

Golovanova, O. A.; Korol'kov, V. V.; Kuimova, M. V.

2017-01-01

The paper presents the features of calcium oxalate crystallization in the presence of additives revealed through experimental modeling. The patterns of phase formation are shown for the Ca2+ - C2O4 2- - H2O and Ca2+ - C2O4 2- - PO4 3- - H2O systems with the components and pH of the saline varying over a wide concentrations range. The effect of additives on crystallization of calcium oxalate monohydrate was investigated. It was found that the ionic strength and magnesium ions are inhibitors, and calcium oxalate and hydroxyapatite crystals are catalysts of calcium oxalate monohydrate crystallization. The basic calcium phosphate (apatite) was found to be most thermodynamically stable, which indicates its special role in kidney stone formation since it is found in virtually all stones.

Growth and electrical properties of (Mn,F) co-doped 0.92Pb(Zn 1/3Nb 2/3)O 3-0.08PbTiO 3 single crystal

NASA Astrophysics Data System (ADS)

Zhang, Shujun; Lebrun, Laurent; Randall, Clive A.; Shrout, Thomas R.

2004-06-01

The growth and characterization of (Mn,F) doped Pb(Zn 1/3Nb 2/3)O 3-PbTiO 3 (PZNT) single crystals are reported in this paper. The typical single crystal obtained is up to 30 mm size with dark brown color. The crystal lattice parameters of doped PZNT crystal are slightly decreased compared to the pure one. The room temperature dielectric permittivity along <0 0 1> direction is about 6000, which is lower than that of the pure PZNT8 because of the dopants. The Curie temperature of the doped crystal is about 180°C while the ferroelectric phase transition temperature is around 100°C, which are higher than those of the pure PZNT8 single crystal. The remnant polarization and coercive field of <0 0 1> oriented doped crystal measured at 1 Hz and 10 kV/cm field are about 27 μC/cm 2 and 4.2 kV/cm, respectively. The room temperature mechanical quality factor is ˜300. Piezoelectric coefficient of <0 0 1> oriented doped crystal is higher than 3500 pC/N and the longitudinal electromechanical coupling factor is larger than 93%. The piezoelectric properties of doped PZNT single crystal with temperature and orientations are also reported in this paper. The valence state of the manganese dopant was determined by electron spin resonance, indicating no Mn 4+ in the crystals, suggesting the valence of manganese ions in PZNT crystals may be 2+, which acts as a hardener, stabilizes the domain wall and pins the domain wall motion, on the other hand, the dopant will enter Ti 4+ position, shifting the crystal composition to higher PT content.

Quantum-chemical insight into structure-reactivity relationship in 4,5,6,7-tetrahalogeno-1H-benzimidazoles: a combined X-ray, DSC, DFT/QTAIM, Hirshfeld surface-based, and molecular docking approach.

PubMed

Latosińska, Jolanta Natalia; Latosińska, Magdalena; Maurin, Jan Krzysztof; Orzeszko, Andrzej; Kazimierczuk, Zygmunt

2014-03-20

The weak interaction patterns in 4,5,6,7-tetrahalogeno-1H-benzimidazoles, protein kinase CK2 inhibitors, in solid state are studied by the X-ray method and quantum chemistry calculations. The crystal structures of 4,5,6,7-tetrachloro- and 4,5,6,7-tetrabromo-1H-benzimidazole are determined by X-ray diffraction and refined to a final R-factor of 3.07 and 3.03%, respectively, at room temperature. The compound 4,5,6,7-tetrabromo-1H-benzimidazole, which crystallizes in the I41/a space group, is found to be isostructural with previously studied 4,5,6,7-tetraiodo-1H-benzimidazole in contrast to 4,5,6,7-tetrachloro-1H-benzimidazole, which crystallizes as triclinic P1̅ with 4 molecules in elementary unit. For 4,5,6,7-tetrachloro-1H-benzimidazole, differential scanning calorimetry (DSC) revealed a second order glassy phase transition at Tg = 95°/106° (heating/cooling), an indication of frozen disorder. The lack of 3D isostructurality found in all 4,5,6,7-tetrahalogeno-1H-benzimidazoles is elucidated on the basis of the intra- and intermolecular interactions (hydrogen bonding, van der Waals contacts, and C-H···π interactions). The topological Bader's Quantum Theory of Atoms in Molecules (QTAIM) and Spackman's Hirshfeld surface-based approaches reveal equilibration of electrostatic matching and dispersion van der Waals interactions between molecules consistent with the crystal site-symmetry. The weakening of van der Waals forces accompanied by increasing strength of the hydrogen bond (N-H···N) result in a decrease in the crystal site-symmetry and a change in molecular packing in the crystalline state. Crystal packing motifs were investigated with the aid of Hirshfeld surface fingerprint plots. The ordering 4,5,6,7-tetraiodo > 4,5,6,7-tetrabromo > 4,5,6,7-tetrachloro > 4,5,6,7-tetrafluoro reflects not only a decrease in crystal symmetry but also increase in chemical reactivity (electronic activation), which could explain some changes in biological activity of compounds from the 4,5,6,7-tetrahalogeno-1H-benzimidazole series. The ability of formation of a given type of bonds by 4,5,6,7-tetrahalogeno-1H-benzimidazole molecules is the same in the crystal and in CK2. Analysis of the interactions in the crystal permits drawing conclusions on the character (the way) of connections between a given 4,5,6,7-tetrahalogeno-1H-benzimidazole as a ligand with CK2 protein to make a protein-ligand complex.

Nanoscale observations of the effect of citrate on calcium oxalate precipitation on calcite surfaces.

NASA Astrophysics Data System (ADS)

Burgos-Cara, Alejandro; Ruiz-Agudo, Encarnacion; Putnis, Christine V.

2016-04-01

Calcium oxalate (CaC2O4ṡxH2O) minerals are naturally occurring minerals found in fossils, plants, kidney stones and is a by-product in some processes such as paper, food and beverage production [1,2]. In particular, calcium oxalate monohydrate phase (COM) also known as whewellite (CaC2O4ṡH2O), is the most frequently reported mineral phase found in urinary and kidney stones together with phosphates. Organic additives are well known to play a key role in the formation of minerals in both biotic and abiotic systems, either facilitating their precipitation or hindering it. In this regard, recent studies have provided direct evidence demonstrating that citrate species could enhance dissolution of COM and inhibit their precipitation. [3,4] The present work aims at evauate the influence of pH, citrate and oxalic acid concentrations in calcium oxalate precipitation on calcite surfaces (Island Spar, Chihuahua, Mexico) through in-situ nanoscale observation using in situ atomic force microscopy (AFM, Multimode, Bruker) in flow-through experiments. Changes in calcium oxalate morphologies and precipitated phases were observed, as well as the inhibitory effect of citrate on calcium oxalate precipitation, which also lead to stabilization an the amorphous calcium oxalate phase. [1] K.D. Demadis, M. Öner, Inhibitory effects of "green"additives on the crystal growth of sparingly soluble salts, in: J.T. Pearlman (Ed.), Green Chemistry Research Trends, Nova Science Publishers Inc., New York, 2009, pp. 265-287. [2] M. Masár, M. Zuborová, D. Kaniansky, B. Stanislawski, Determination of oxalate in beer by zone electrophoresis on a chip with conductivity detection, J. Sep. Sci. 26 (2003) 647-652. [3] Chutipongtanate S, Chaiyarit S, Thongboonkerd V. Citrate, not phosphate, can dissolve calcium oxalate monohydrate crystals and detach these crystals from renal tubular cells. Eur J Pharmacol 2012;689:219-25. [4] Weaver ML, Qiu SR, Hoyer JR, Casey WH, Nancollas GH, De Yoreo JJ. Inhibition of calcium oxalate monohydrate growth by citrate and the effect of the background electrolyte. J Cryst Growth 2007;306:135-45.

Investigation of the crystallization features, atomic structure, and microstructure of chromium-doped monticellite

NASA Astrophysics Data System (ADS)

Subbotin, K. A.; Iskhakova, L. D.; Zharikov, E. V.; Lavrishchev, S. V.

2008-12-01

A series of Cr4+:CaMgSiO4 single crystals is grown using floating zone melting, and their microstructure, composition, and crystal structure are investigated. It is shown that regions with inclusions of second phases, such as forsterite, akermanite, MgO, and Ca4Mg2Si3O12, can form over the length of the sample. The composition of the single-phase regions of the single crystals varies from the stoichiometric monticellite CaMgSiO4 to the solid solution Ca(1 - x)Mg(1 + x)SiO4( x = 0.22). The Cr:(Ca0.88Mg0.12)MgSiO4 crystal is studied using X-ray diffraction. It is revealed that, in this case, the olivine-like orthorhombic crystal lattice is distorted to the monoclinic lattice with the parameters a = 6.3574(5) Å, b = 4.8164(4) Å, c = 11.0387(8) Å, β = 90.30(1)o, Z = 4, V = 337.98 Å3, and space group P21/ c. In the monoclinic lattice, the M(1) position of the initial olivine structure is split into two nonequivalent positions with the center of symmetry, which are occupied only by Mg2+ cations with the average length of the Mg-O bond R av = 2.128 Å. The overstoichiometric Mg2+ cations partially replace Ca2+ cations (in the M(2) position of the orthorhombic prastructure) with the average bond length of 2.347 Å in the [(Ca,Mg)-O6] octahedron. The average distance in SiO4 distorted tetrahedra is 1.541 Å.

The perfection and defect structure of organic hourglass inclusion K 2SO 4 crystals

NASA Astrophysics Data System (ADS)

Vetter, William M.; Totsuka, Hirono; Dudley, Michael; Kahr, Bart

2002-06-01

Hourglass inclusion crystals of K 2SO 4 were grown from aqueous solutions containing the dye acid fuchsin, and studied by synchrotron white-beam X-ray topography and reciprocal space mapping. Both self-nucleated and larger, seeded dye-included crystals were prepared, as well as comparable undoped crystals. While the dye modified the crystals' habit strongly, X-ray topographs showed it had no influence on their dislocation configurations, which were typical for solution-grown crystals. No kinematical contrast arising from the presence of the dye was observed that indicated dye-induced strain in the crystal lattice. Growth sector boundaries were visible in the dyed crystals but not in undoped crystals, implying there was a slightly higher lattice mismatch across growth sector boundaries in the dye-included crystals. Reciprocal space maps of small areas on an hourglass inclusion crystal within either a dye-included growth sector or an undoped growth sector showed single peaks with the same perfect crystal rocking curve width and no dilatation or tilt of the host lattice resulting from the dye's presence. These results showed hourglass inclusion crystals can be grown in which the presence of the dye disturbs the crystalline structure of the host salt minimally, and that hourglass inclusions have the nature of a solid solution.

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

Bolotin, B. M., E-mail: bolotin70@yandex.ru; Mikhlina, Ya. A.; Arkhipova, S. A.

The crystal and molecular structures of two crystal forms (pale yellow form 1 and yellow form 2) of N-[2-(4-oxo-4H-benzo[d][1,3]oxazin-2-yl)phenyl]naphthalene-2-sulfonamide (Orlyum White 520T), which is an organic luminophore with an anomalously high Stokes shift, were determined. Crystal 2 is a solvate with para-xylene. Crystal 1 is a solvent-free form. The molecular geometry in crystal 1 differs from that in 2 only in the orientation of the SO{sub 2}Ar substituent. The bond-length distribution in the planar moiety of the molecule in crystal 1 is virtually identical to that in 2, but the bonds in the NH-SO{sub 2}Ar-bearing benzene ring in crystal 1more » are systematically longer than the corresponding bonds in crystal 2. This fact can be attributed to the crystal-packing effects. In 2 the molecules form stacked dimers with {pi}-stacking interactions between two planar conjugated tricyclic systems. The charge transfer in this system accounts for the intensification of the color of these crystals and the observed difference in the optical properties of 1 and 2.« less

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

PubMed

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

2014-03-17

A new framework cobalt(II) hydroxyl phosphate, Co2PO4OH, was prepared by ionothermal synthesis using 1-butyl-4-methyl-pyridinium hexafluorophosphate as the ionic liquid. As the formation of Co2PO4F competes in the synthesis, the synthesis conditions have to be judiciously chosen to obtain well-crystallized, single phase Co2PO4OH. Single-crystal X-ray diffraction analyses reveal Co2PO4OH crystallizes with space group I41/amd (a = b = 5.2713(7) Å, c = 12.907(3) Å, V = 358.63(10) Å(3), and Z = 4). Astonishingly, it does not crystallize isotypically with Co2PO4F but rather isotypically with the hydroxyl minerals caminite Mg1.33[SO4(OH)0.66(H2O)0.33] and lipscombite Fe(2–y)PO4(OH) (0 ≤ y ≤ 2/3). Phosphate tetrahedra groups interconnect four rod-packed face-sharing ∞(1){CoO(6/2)} octahedra chains to form a three-dimensional framework structure. The compound Co2PO4OH was further characterized by powder X-ray diffraction, Fourier transform–infrared, and ultraviolet–visible spectroscopy, confirming the discussed structure. The magnetic measurement reveals that Co2PO4OH undergoes a magnetic transition and presents at low temperatures a canted antiferromagnetic spin order in the ground state.

Crystal growth methods dedicated to low solubility actinide oxalates

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

Tamain, C., E-mail: christelle.tamain@cea.fr; Arab-Chapelet, B.; Rivenet, M.

Two novel crystal growth syntheses dedicated to low solubility actinide-oxalate systems and adapted to glove box handling are described. These methods based on the use of precursors of either actinide metal or oxalic acid have been optimized on lanthanide systems (analogue of actinides(III)) and then assessed on real actinide systems. They allow the synthesis of several actinide oxalate single crystals, Am{sub 2}(C{sub 2}O{sub 4}){sub 3}(H{sub 2}O){sub 3}·xH{sub 2}O, Th(C{sub 2}O{sub 4}){sub 2}·6H{sub 2}O, M{sub 2+x}[Pu{sup IV}{sub 2−x}Pu{sup III}{sub x}(C{sub 2}O{sub 4}){sub 5}]·nH{sub 2}O and M{sub 1−x}[Pu{sup III}{sub 1−x}Pu{sup IV}{sub x}(C{sub 2}O{sub 4}){sub 2}·H{sub 2}O]·nH{sub 2}O. It is the first timemore » that these well-known compounds are formed by crystal growth methods, thus enabling direct structural studies on transuranic element systems and acquisition of basic data beyond deductions from isomorphic (or not) lanthanide compounds. Characterizations by X-ray diffraction, UV–visible solid spectroscopy, demonstrate the potentialities of these two crystal growth methods to obtain oxalate compounds. - Graphical abstract: Two new single crystal growth methods dedicated to actinide oxalate compounds. - Highlights: • Use of diester as oxalate precursor for crystal growth of actinide oxalates. • Use of actinide oxide as precursor for crystal growth of actinide oxalates. • Crystal growth of Pu(III) and Am(III) oxalates. • Crystal growth of mixed Pu(III)/Pu(IV) oxalates.« less

Growth and characterization of pure and Ca2+ doped MnHg(SCN)4 single crystals

NASA Astrophysics Data System (ADS)

Latha, C.; Mahadevan, C. K.; Guo, Li; Liu, Jinghe

2018-05-01

Manganese-mercury thiocyanate, MnHg(SCN)4, crystal is considered to be an important organometallic nonlinear optical (NLO) material exhibiting higher thermal stability and second harmonic generation (SHG) efficiency. In order to understand the effect of Ca2+ as an impurity on the physicochemical properties, we have grown pure and Ca2+ doped (with a concentration of 1 mol%) MnHg(SCN)4 single crystals by the free evaporation of solvent method and characterized structurally, chemically, optically and electrically by adopting the available standard methods. Results obtained indicate that Ca2+ doping increases significantly the optical transmittance, SHG efficiency, and DC electrical conductivity and decreases the dielectric loss factor (improves the crystal quality), and AC electrical conductivity without distorting the crystal structure. Also, the low dielectric constant (εr) values observed for both the pure and doped crystals considered at near ambient temperatures indicate the possibility of using these crystals not only as potential NLO materials (useful in the photonics industry) but also as promising low εr value dielectric materials (useful in the microelectronics industry).

Diode-pumped quasi-three-level Nd:GdV O4-Nd:YAG sum-frequency laser at 464 nm

NASA Astrophysics Data System (ADS)

Lu, Jie

2014-04-01

We report a laser architecture to obtain continuous-wave (cw) blue radiation at 464 nm. A 808 nm diode pumped a Nd:GdV O4 crystal emitting at 912 nm. A part of the pump power was then absorbed by the Nd:GdV O4 crystal. The remainder was used to pump a Nd:YAG crystal emitting at 946 nm. Intracavity sum-frequency mixing at 912 and 946 nm was then realized in a LiB3O5 (LBO) crystal to produce blue radiation. We obtained a cw output power of 1.52 W at 464 nm with a pump laser diode emitting 18.4 W at 808 nm.

Magnetic anisotropy and spin-flop transition of NiWO4 single crystals

NASA Astrophysics Data System (ADS)

Liu, C. B.; He, Z. Z.; Liu, Y. J.; Chen, R.; Shi, M. M.; Zhu, H. P.; Dong, C.; Wang, J. F.

2017-12-01

NiWO4 exhibits a spin chain structure built by magnetic Ni2+ ions, which may be considered as a one dimensional S = 1 system. In this work, large-sized single crystals of NiWO4 were successfully synthesized by a flux method and the crystal quality was confirmed by X-ray diffraction. Magnetic properties of obtained single crystals were studied by means of magnetic susceptibility and high field magnetization along crystallographic axes. The results demonstrate that NiWO4 is highly magnetic anisotropic and possesses a three-dimensional long range ordering below 60 K, where a spin flop transition can be observed at 17.5 T in applied magnetic fields along the magnetic easy axis (c-axis).

One dimensional coordination polymers: Synthesis, crystal structures and spectroscopic properties

NASA Astrophysics Data System (ADS)

Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla; Şenyel, Mustafa; Şahin, Onur

2016-11-01

Two new one dimensional (1D) cyanide complexes, namely [M(4-aepy)2(H2O)2][Pt(CN)4], (4-aepy = 4-(2-aminoethyl)pyridine M = Cu(II) (1) or Zn(II) (2)), have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal and elemental analyses techniques. The crystallographic analyses reveal that 1 and 2 are isomorphous and isostructural, and crystallize in the monoclinic system and C2 space group. The Pt(II) ions are coordinated by four cyanide-carbon atoms in the square-planar geometry and the [Pt(CN)4]2- ions act as a counter ion. The M(II) ions display an N4O2 coordination sphere with a distorted octahedral geometry, the nitrogen donors belonging to four molecules of the organic 4-aepy that act as unidentate ligands and two oxygen atoms from aqua ligands. The crystal structures of 1 and 2 are similar each other and linked via intermolecular hydrogen bonding, Pt⋯π interactions to form 3D supramolecular network. Vibration assignments of all the observed bands are given and the spectral features also supported to the crystal structures of the complexes.

Synthesis, growth, structural, thermal and optical studies of pyrrolidinium-2-carboxylate-4-nitrophenol single crystals.

PubMed

Swarna Sowmya, N; Sampathkrishnan, S; Vidyalakshmi, Y; Sudhahar, S; Mohan Kumar, R

2015-06-15

Organic nonlinear optical material, pyrrolidinium-2-carboxylate-4-nitrophenol (PCN) was synthesized and single crystals were grown by slow evaporation solution growth method. Single crystal X-ray diffraction analysis confirmed the structure and lattice parameters of PCN crystals. Infrared, Raman and NMR spectral analyses were used to elucidate the functional groups present in the compound. The thermal behavior of synthesized compound was studied by thermogravimetric and differential scanning calorimetry (TG-DSC) analyses. The photoluminescence property was studied by exciting the crystal at 360 nm. The relative second harmonic generation (SHG) efficiency of grown crystal was estimated by using Nd:YAG laser with fundamental wavelength of 1,064 nm. Copyright © 2015 Elsevier B.V. All rights reserved.

From crystal morphology to molecular and scale crystallography

NASA Astrophysics Data System (ADS)

Janner, A.; Janssen, T.

2015-08-01

A number of topics, ranging from morphology of aperiodic crystals to indexed enclosing forms of axial-symmetric proteins, nucleic acids and viruses, have been selected among those investigated by the authors in 50 years of research. The basic symmetries involved in fields like superspace, molecular and scale crystallography, are considered from a personal point of view in their time evolution. A number of specific subjects follow, chosen among a few highlights and presented according to the experience of the authors: snow crystals, calaverite {{AuTe}}2, the incommensurately modulated crystals {{Rb}}2{{ZnBr}}4, {[{N}{({{CH}}3)}4]}2{{ZnCl}}4 and the mitochondrial ferritin.

Li2MoO4 crystal growth from solution activated by low-frequency vibrations

NASA Astrophysics Data System (ADS)

Barinova, Olga; Sadovskiy, Andrey; Ermochenkov, Ivan; Kirsanova, Svetlana; Sukhanova, Ekaterina; Kostikov, Vladimir; Belov, Stanislav; Mozhevitina, Elena; Khomyakov, Andrew; Kuchuk, Zhanna; Zharikov, Eugeny; Avetissov, Igor

2017-01-01

The possibility of Li2MoO4 crystal growth from aqueous solutions activated by axial vibrational control (AVC) technique was investigated. It was found out that a low-frequency mechanical activation of the solution led to an increase of Li2MoO4 equilibrium solubility in aqueous solution for 11 rel% in the 25-29 °C temperature range. The changes in solution structure were analyzed in situ by Raman study of the solution. The AVC activation of solution resulted in a re-faceting of growing crystals, a smoothing of a face surface morphology and reduction of water content in the crystal.

The Crystal and Molecular Structure of Acetatochlorobis(4-methylpyridine)oxovanadium (IV)

NASA Technical Reports Server (NTRS)

Schupp, John D.; Hepp, Aloysius F.; Duraj, Stan A.; Richman, Robert M.; Fanwick, Phillip E.; Hakimzadeh, Roshanak (Technical Monitor)

2001-01-01

The crystal and molecular structure of the title compound, VOCl(O2CCH3)(4-CH3C5H4N)2, has been determined by single-crystal x-ray diffraction. The material crystallizes in the space group P 1(bar) (#2) with a = 7.822(2), b = 8.023(l), c = 14.841(2) Angstroms, alpha = 99.73(l), beta = 91.41(l), and gamma = 117.13(l). The coordination geometry around the vanadium is a highly distorted octahedron. The molecule is remarkable for being a monomeric oxovanadium (IV) carboxylate. A generalized synthetic strategy is proposed for the preparation of oxovanadium (IV) monomers.

The influence of impurities on phosphoric acid hemihydrate crystallization

NASA Astrophysics Data System (ADS)

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

2007-09-01

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

Purification, crystallization and preliminary crystallographic study of an IDS-epimerase from Agrobacterium tumefaciens BY6

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

Bäuerle, Bettina; Sandalova, Tatyana; Schneider, Gunter

2006-08-01

This is the first report of the crystallization of an IDS-epimerase from A. tumefaciens BY6 and its l-selenomethionine derivative. The initial degradation of all stereoisomers of the complexing agent iminodisuccinate (IDS) is enabled by an epimerase in the bacterial strain Agrobacterium tumefaciens BY6. This protein was produced in Escherichia coli, purified and crystallized by the hanging-drop vapour-diffusion method. Crystals of IDS-epimerase were obtained under several conditions. The best diffracting crystals were grown in 22% PEG 3350, 0.2 M (NH{sub 4}){sub 2}SO{sub 4} and 0.1 M bis-Tris propane pH 7.2 at 293 K. These crystals belong to the monoclinic space groupmore » P2{sub 1}, with unit-cell parameters a = 55.4, b = 104.2, c = 78.6 Å, β = 103.3°, and diffracted to 1.7 Å resolution. They contain two protein molecules per asymmetric unit. In order to solve the structure using the MAD phasing method, crystals of the l-selenomethionine-substituted epimerase were grown in the presence of 20% PEG 3350, 0.2 M Na{sub 2}SO{sub 4} and 0.1 M bis-Tris propane pH 8.5.« less

Struvite formation and decomposition characteristics for ammonia and phosphorus recovery: A review of magnesium-ammonia-phosphate interactions.

PubMed

Tansel, Berrin; Lunn, Griffin; Monje, Oscar

2018-03-01

Struvite (MgNH 4 PO 4 ·6H 2 O) forms in aqueous systems with high ammonia and phosphate concentrations. However, conditions that result into struvite formation are highly dependent on the ionic compositions, temperature, pH, and ion speciation characteristics. The primary ions involved in struvite formation have complex interactions and can form different crystals depending on the ionic levels, pH and temperature. Struvite as well as struvite analogues (with substitution of monovalent cations for NH 4 + or divalent cations for Mg 2+ ) as well as other crystals can form simultaneously and result in changes in crystal morphology during crystal growth. This review provides the results from experimental and theoretical studies on struvite formation and decomposition studies. Characteristics of NH 4 + or divalent cations for Mg 2+ were evaluated in comparison to monovalent and divalent ions for formation of struvite and its analogues. Struvite crystals forming in wastewater systems are likely to contain crystals other than struvite due to ionic interactions, pH changes, temperature effects and clustering of ions during nucleation and crystal growth. Decomposition of struvite occurs following a series of reactions depending on the rate of heating, temperature and availability of water during heating. Copyright © 2017 Elsevier Ltd. All rights reserved.

New materials for high-energy-resolution x-ray optics

DOE PAGES

Yavas, Hasan; Sutter, John P.; Gog, Thomas; ...

2017-06-09

The use of crystals other than silicon for x-ray optics is becoming more common for many challenging experiments such as resonant inelastic x-ray scattering and nuclear resonant scattering. As more—and more specialized—spectrometers become available at many synchrotron radiation facilities, interest in pushing the limits of experimental energy resolution has increased. The potentially large improvements in resolution and efficiency that nonsilicon optics offer are beginning to be realized. Furthermore, this article covers the background and state of the art for nonsilicon crystal optics with a focus on a resolution of 10 meV or better, concentrating on compounds that form trigonal crystals,more » including sapphire, quartz, and lithium niobate, rather than the more conventional cubic materials, including silicon, diamond, and germanium.« less

A spatially resolving x-ray crystal spectrometer for measurement of ion-temperature and rotation-velocity profiles on the Alcator C-Mod tokamak.

PubMed

Hill, K W; Bitter, M L; Scott, S D; Ince-Cushman, A; Reinke, M; Rice, J E; Beiersdorfer, P; Gu, M-F; Lee, S G; Broennimann, Ch; Eikenberry, E F

2008-10-01

A new spatially resolving x-ray crystal spectrometer capable of measuring continuous spatial profiles of high resolution spectra (lambda/d lambda>6000) of He-like and H-like Ar K alpha lines with good spatial (approximately 1 cm) and temporal (approximately 10 ms) resolutions has been installed on the Alcator C-Mod tokamak. Two spherically bent crystals image the spectra onto four two-dimensional Pilatus II pixel detectors. Tomographic inversion enables inference of local line emissivity, ion temperature (T(i)), and toroidal plasma rotation velocity (upsilon(phi)) from the line Doppler widths and shifts. The data analysis techniques, T(i) and upsilon(phi) profiles, analysis of fusion-neutron background, and predictions of performance on other tokamaks, including ITER, will be presented.

Significantly different pulse shapes for γ- and α-rays in Gd3Al2Ga3O12:Ce3+ scintillating crystals

NASA Astrophysics Data System (ADS)

Kobayashi, Masaaki; Tamagawa, Yoichi; Tomita, Shougo; Yamamoto, Akihiro; Ogawa, Izumi; Usuki, Yoshiyuki

2012-12-01

We have found that scintillation in Gd3Al2Ga3O12 (GAGG):Ce3+ garnet single crystals has significantly different pulse shapes for 0.662 MeV γ- and 5.47 MeV α-rays. The decay and rise times for γ-rays are smaller by 50% and threefold, respectively, than those for α-rays. Because the GAGG:Ce is a dense, efficient and fast-response scintillator and because it can be grown in large-size single crystals, it should be a promising unified target and a detector material in the study of neutrinoless double beta decay of 160Gd through the use of pulse shape discrimination between the β-ray signals and the α-ray-induced backgrounds.

Expression, purification and crystallization of Streptococcus dysgalactiae-derived mitogen

PubMed Central

Papageorgiou, Anastassios C.; Saarinen, Susanna; Ramirez-Bartutis, Rosa; Kato, Hidehito; Uchiyama, Takehiko; Kirikae, Teruo; Miyoshi-Akiyama, Toru

2006-01-01

Superantigens are bacterial or viral toxins with potent immunostimulatory properties. Streptococcus dysgalactiae-derived mitogen, a 25 kDa protein, is a recently discovered superantigen isolated from S. dysgalactiae culture supernatant. Sequence considerations suggest that it belongs to a new superantigen family distinct from other superantigens. The protein was expressed in Escherichia coli cells and purified to homogeneity. Crystals were grown at pH 4.2–4.4 in the presence of 18–20%(w/v) PEG 3350 and 0.4 M lithium nitrate. A complete data set to 2.4 Å resolution was collected from a single crystal at liquid-nitrogen temperatures using synchrotron radiation. The crystals belong to space group P3/P31/P32, with unit-cell parameters a = b = 52.7, c = 62.4 Å, γ = 120° and one molecule in the crystallographic asymmetric unit. PMID:16511312

Composition effect in luminescence properties of Y(NbxTa1-x)O4 mixed crystals

NASA Astrophysics Data System (ADS)

Spassky, D.; Vasil'ev, A.; Vielhauer, S.; Sidletskiy, O.; Voloshyna, O.; Belsky, A.

2018-06-01

The luminescence properties of Y(NbxTa1-x)O4 mixed crystals were studied. Local structure modifications arise due to the inhomogeneous distribution of the substitutional ions in the mixed crystal and can be traced using the luminescence spectroscopy. In particular, it is shown that the intensity of exciton emission under interband VUV excitation increases for intermediate values of x with the maximum at x = 0.4 relatively to the intensity observed in the constituents of the mixed crystals - YTaO4 and YNbO4. From the luminescence excitation spectra it follows that the probability of exciton creation from the separated e-h pairs increases for intermediate values of x as well. Using numerical simulation it is shown that the effect is connected with the variation of the thermalization length of hot electrons and holes, which is minimal at x = 0.4.

Fluorescent Approaches to High Throughput Crystallography

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Forsythe, Elizabeth; Achari, Aniruddha

2006-01-01

We have shown that by covalently modifying a subpopulation, less than or equal to 1%, of a macromolecule with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of purification, and the presence of the probe at low concentrations does not affect the X-ray data quality or the crystallization behavior. The presence of the trace fluorescent label gives a number of advantages when used with high throughput crystallizations. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination crystals show up as bright objects against a dark background. Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Brightly fluorescent crystals are readily found against less bright precipitated phases, which under white light illumination may obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries as the protein or protein structures is all that shows up. Fluorescence intensity is a faster search parameter, whether visually or by automated methods, than looking for crystalline features. We are now testing the use of high fluorescence intensity regions, in the absence of clear crystalline features or "hits", as a means for determining potential lead conditions. A working hypothesis is that kinetics leading to non-structured phases may overwhelm and trap more slowly formed ordered assemblies, which subsequently show up as regions of brighter fluorescence intensity. Preliminary experiments with test proteins have resulted in the extraction of a number of crystallization conditions from screening outcomes based solely on the presence of bright fluorescent regions. Subsequent experiments will test this approach using a wider range of proteins. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons.

Crystal growth and optical properties of 4-aminobenzophenone (ABP)

NASA Astrophysics Data System (ADS)

Li, Zhengdong; Wu, Baichang; Su, Genbo; Huang, Gongfan

1997-02-01

Bulk crystals of 4-aminobenzophenone (ABP) were grown from organic solution. The crystal structure was determined by X-ray analysis. The refractive indices were determined by the method of prism minimum deviation. Some effective nonlinear-optical coefficients deff were measured. A blue second-harmonic emission with wavelengths of 433 and 460 nm were observed during laser diode pumping.

Antiurolithic activity of Origanum vulgare is mediated through multiple pathways

PubMed Central

2011-01-01

Background Origanum vulgare Linn has traditionally been used in the treatment of urolithiasis. Therefore, we investigated the crude extract of Origanum vulgare for possible antiurolithic effect, to rationalize its medicinal use. Methods The crude aqueous-methanolic extract of Origanum vulgare (Ov.Cr) was studied using the in vitro and in vivo methods. In the in vitro experiments, supersaturated solution of calcium and oxalate, kidney epithelial cell lines (MDCK) and urinary bladder of rabbits were used, whereas, in the in vivo studies, rat model of urolithiasis was used for the study of preventive and curative effect. Results In the in vitro experiments, Ov.Cr exhibited a concentration-dependent (0.25-4 mg/ml) inhibitory effect on the slope of nucleation and aggregation and also decreased the number of calcium oxalate monohydrate crystals (COM) produced in calcium oxalate metastable solutions. It also showed concentration-dependent antioxidant effect against DPPH free radical and lipid peroxidation induced in rat kidney tissue homogenate. Ov.Cr reduced the cell toxicity using MTT assay and LDH release in renal epithelial cells (MDCK) exposed to oxalate (0.5 mM) and COM (66 μg/cm2) crystals. Ov.Cr relaxed high K+ (80 mM) induced contraction in rabbit urinary bladder strips, and shifted the calcium concentration-response curves (CRCs) towards right with suppression of the maximum response similar to that of verapamil, a standard calcium channel blocker. In male Wistar rats receiving lithogenic treatment comprising of 0.75% ethylene glycol in drinking water given for 3 weeks along with ammonium chloride (NH4Cl) for the first 5 days, Ov.Cr treatment (10-30 mg/kg) prevented as well as reversed toxic changes including loss of body weight, polyurea, crystalluria, oxaluria, raised serum urea and creatinine levels and crystal deposition in kidneys compared to their respective controls. Conclusion These data indicating the antiurolithic activity in Ov.Cr, possibly mediated through inhibition of CaOx crystallization, antioxidant, renal epithelial cell protective and antispasmodic activities, rationalizes its medicinal use in urolithiasis. PMID:22004514

Multidisciplinary Approaches to Radiation Balanced Lasers (MARBLe): 1st Annual Progress Report

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

Hehlen, Markus Peter

The initial main modifications of the existing μPD crystal-growth system at LANL have been completed. This now gives us the new capability to develop the growth of crystalline RBL materials by both the μPD and the Bridgman method. Quantitative mass spectrometry of the growth atmosphere was conducted to identify possible sources of gaseous trace species (primarily hydrogen) that could cause the undesired reduction of Yb 3+ to Yb 2+ during the crystal growth. Hydrogen was found to be at sufficiently low levels to not be a respective concern. Studies on the thermal decomposition of YbF 3 to form Yb 2+more » are currently underway in collaboration with MARBLe team member Prof. Pauzauskie. First samples of Yb 3+-doped YLiF 4 (YLF:Yb) and undoped LiLuF 4 (LLF) were grown, and MARBLe team member Prof. Sheik-Bahae has performed measurements of laser-induced heating (YLF:Yb) and background absorption coefficient (LLF). We discovered that one or several of the YF 3, LiF, and YbF 3 precursors contains organic impurities that chemically reduce to black residue during the high-temperature growth in oxygen-free argon atmosphere. A process for removal of these residues prior to growth is being considered. Comparing the results from incongruently melting YLF with those of congruently melting LLF indicate that a congruently melting material is preferred for Bridgman growth. Crystal-growth experiments with LLF are currently underway. The results of these studies on Yb 3+ doped materials will be directly applicable to the future growth of Er 3+ and Tm 3+ doped as well as Yb 3+, Nd 3+ co-doped RBL crystals. There was no activity on the parallel effort of developing rareearth- doped chalcogenide glasses. The primary reason was a lack of manpower due to a delayed hiring of a student. In September 2017, we have hired a Postdoctoral Researcher who will be able to contribute to the growth (at LANL) and optical characterization (at UNM) of RBL materials.« less

Growth and optical waveguide fabrication in spinel MgGa2O4 crystal

NASA Astrophysics Data System (ADS)

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

2017-10-01

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

Melt growth of zinc aluminate spinel single crystal by the micro-pulling down method under atmospheric pressure

NASA Astrophysics Data System (ADS)

Kamada, K.; Shoji, Y.; Yamaji, A.; Kurosawa, S.; Yokota, Yuui; Ohashi, Y.; Kim, Kyoung Jin; Ivanov, M.; Kochurikhin, V. V.; Yoshikawa, A.

2018-06-01

ZnAl2O4 crystals were grown using few starting compositions with various ZnO:AlO3/2 ratio using an Ir wire seed and Ir + Re crucible under ordinary pressure with Ar + 2%O2 atmosphere by the radiofrequency heating μ-PD furnace. The ZnAl2O4 spinel single crystal with 4 mm diameter could be successfully grown by the μ-PD method by optimization of starting melt composition considering with Zinc oxide evaporation. During 10 min of growth under normal pressure the formation of ZnAl2O4 single phase observed even at high vapor pressure of ZnO. The transmittance spectra and X-ray locking curve were measured for evaluating of grown ZnAl2O4 crystals quality.

Thickness distributions and evolution of growth mechanisms of NH4-illite from the fossil hydrothermal system of Harghita Bai, Eastern Carpathians, Romania

USGS Publications Warehouse

Bobos, Iuliu; Eberl, Dennis D.

2013-01-01

The crystal growth of NH4-illite (NH4-I) from the hydrothermal system of Harghita Bãi (Eastern Carpathians) was deduced from the shapes of crystal thickness distributions (CTDs). The 4-illite-smectite (I-S) interstratified structures (R1, R2, and R3-type ordering) with a variable smectite-layer content. The NH4-I-S (40–5% S) structures were identified underground in a hydrothermal breccia structure, whereas the K-I/NH4-I mixtures were found at the deepest level sampled (−110 m). The percentage of smectite interlayers generally decreases with increasing depth in the deposit. This decrease in smectite content is related to the increase in degree of fracturing in the breccia structure and corresponds to a general increase in mean illite crystal thickness. In order to determine the thickness distributions of NH4-I crystals (fundamental illite particles) which make up the NH4-I-S interstratified structures and the NH4,-I/K-I mixtures, 27 samples were saturated with Li+ and aqueous solutions of PVP-10 to remove swelling and then were analyzed by X-ray diffraction. The profiles for the mean crystallite thickness (Tmean) and crystallite thickness distribution (CTD) of NH4-I crystallites were determined by the Bertaut-Warren-Averbach method using the MudMaster computer code. The Tmean of NH4-I from NH4-I-S samples ranges from 3.4 to 7.8 nm. The Tmean measured for the NH4-I/K-I mixture phase ranges from 7.8 nm to 11.7 nm (NH4-I) and from 12.1 to 24.7 nm (K-I).The CTD shapes of NH4-I fundamental particles are asymptotic and lognormal, whereas illites from NH4-I/K-I mixtures have bimodal shapes related to the presence of two lognormal-like CTDs corresponding to NH4-I and K-I.The crystal-growth mechanism for NH4-I samples was simulated using the Galoper code. Reaction pathways for NH4-I crystal nucleation and growth could be determined for each sample by plotting their CTD parameters on an α–β2 diagram constructed using Galoper. This analysis shows that NH4-I crystals underwent simultaneous nucleation and growth, followed by surface-controlled growth without simultaneous nucleation.

Recent developments in the growth, processing, and testing of rare earth doped YVO{sub 4} single crystals

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

Mizell, G.; Fay, W.R.; Alekel, T. III

1994-12-31

The production of the laser host material YVO{sub 4} via high temperature solution growth (HTSG) is described as a facile alternative for producing optical quality crystals for research. The effects of dopant concentration on optical absorption properties in 0.7% and 3% Nd:YVO{sub 4} crystals are discussed. The rare earths ions Ho{sup 3+} and Er{sup 3+} have been doped into YVO{sub 4} with the HTSG method, and inaugural optical properties of Ho{sub 0.04}Y{sub 0.96}VO{sub 4} are presented.

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

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

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

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

Tunable photonic crystals with partial bandgaps from blue phase colloidal crystals and dielectric-doped blue phases.

PubMed

Stimulak, Mitja; Ravnik, Miha

2014-09-07

Blue phase colloidal crystals and dielectric nanoparticle/polymer doped blue phases are demonstrated to combine multiple components with different symmetries in one photonic material, creating a photonic crystal with variable and micro-controllable photonic band structure. In this composite photonic material, one contribution to the band structure is determined by the 3D periodic birefringent orientational profile of the blue phases, whereas the second contribution emerges from the regular array of the colloidal particles or from the dielectric/nanoparticle-doped defect network. Using the planewave expansion method, optical photonic bands of the blue phase I and II colloidal crystals and related nanoparticle/polymer doped blue phases are calculated, and then compared to blue phases with no particles and to face-centred-cubic and body-centred-cubic colloidal crystals in isotropic background. We find opening of local band gaps at particular points of Brillouin zone for blue phase colloidal crystals, where there were none in blue phases without particles or dopants. Particle size and filling fraction of the blue phase defect network are demonstrated as parameters that can directly tune the optical bands and local band gaps. In the blue phase I colloidal crystal with an additionally doped defect network, interestingly, we find an indirect total band gap (with the exception of one point) at the entire edge of SC irreducible zone. Finally, this work demonstrates the role of combining multiple - by symmetry - differently organised components in one photonic crystal material, which offers a novel approach towards tunable soft matter photonic materials.

Large Ice Crystal Charge Transfer Studies

DTIC Science & Technology

1988-10-28

electrification. However, the extra- polation using qcd 4 was completely unjustified. With corrected values of the separation probability of ice crystals...contact to leak away from the local area or become trapped in the crystal lattice . Obviously, larger initial charge transfers, with larger 6 crystals

Protein Crystal Based Nanomaterials

NASA Technical Reports Server (NTRS)

Bell, Jeffrey A.; VanRoey, Patrick

2001-01-01

This is the final report on a NASA Grant. It concerns a description of work done, which includes: (1) Protein crystals cross-linked to form fibers; (2) Engineering of protein to favor crystallization; (3) Better knowledge-based potentials for protein-protein contacts; (4) Simulation of protein crystallization.

Crystalline inclusions in the cytoplasm and nuclei of cells of acute myeloid leukaemia.

PubMed

Pearson, E C

1989-01-01

In a survey by electron microscopy of peripheral blood and/or bone marrow from 230 adult patients with acute myeloid leukaemia, five were observed to contain crystalline inclusions in the cytoplasm of the leukaemic cells and a sixth contained crystals in the nuclei. In four cases, two of FAB type M2 and two of M4, the cytoplasmic crystals were hexagonal in section and 1-2 micron long. Two examples showed internal periodicities in the range 3.3-4.0 nm when the electronmicrographs were analysed by optical diffractometry. A single case of M1 contained smaller trapezoidal crystals with a 4.9nm periodicity. The sixth patient, with unusual cytological abnormalities and a rare t(3; 6) chromosomal translocation, contained six-sided crystals in the nuclei of some relatively undifferentiated cells. To the best of our knowledge such intranuclear crystals have not previously been reported in leukaemia. The relevance of the crystals to the leukaemic process is discussed.

Thermal response, catalytic activity, and color change of the first hybrid vanadate containing Bpe guest molecules.

PubMed

Fernández de Luis, Roberto; Urtiaga, M Karmele; Mesa, José L; Larrea, Edurne S; Iglesias, Marta; Rojo, Teófilo; Arriortua, María I

2013-03-04

Four isomorphic compounds with formula [{Co2(H2O)2(Bpe)2}(V4O12)]·4H2O·Bpe, CoBpe 1; [{CoNi(H2O)2(Bpe)2}(V4O12)]·4H2O·Bpe, CoNiBpe 2; [{Co0.6Ni1.4(H2O)2(Bpe)2}(V4O12)]·4H2O·Bpe, NiCoBpe 3; and [{Ni2(H2O)2(Bpe)2}(V4O12)]·4H2O·Bpe, NiBpe 4, have been obtained by hydrothermal synthesis. The crystal structures of CoBpe 1 and NiBpe 4 were determined by single-crystal X-ray diffraction (XRD). The Rietveld refinement of CoNiBpe 2 and NiCoBpe 3 XRD patterns confirms that those are isomorphic. The compounds crystallize in the P1̅ space group, exhibiting a crystal structure constructed from inorganic layers pillared by Bpe ligands. The crystal structure contains intralayer and interlayer channels, in which the crystallization water molecules and Bpe guest molecules, respectively, are located. The solvent molecules establish a hydrogen bonding network with the coordinated water molecules. Thermodiffractometric and thermogravimetric studies showed that the loss of crystallization and coordinated water molecules takes place at different temperatures, giving rise to crystal structure transformations that involve important reduction of the interlayer distance, and strong reduction of crystallinity. The IR, Raman, and UV-vis spectra of the as-synthesized and heated compounds confirm that the structural building blocks and octahedral coordination environment of the metal centers are maintained after the structural transformations. The color change and reversibility of the water molecules uptake/removal were tested showing that the initial color is not completely recovered when the compounds are heated at temperatures higher than 200 °C. The thermal evolution of the magnetic susceptibility indicates one-dimensional antiferromagnetic coupling of the metal centers at high temperatures. For NiCoBpe 3 and NiBpe 4 compounds magnetic ordering is established at low temperatures, as can be judged by the maxima observed in the magnetic susceptibilities. CoNiBpe 2 was proved as catalyst being active for cyanosilylation reactions of aldehydes.

Easy methods to study the smart energetic TNT/CL-20 co-crystal.

PubMed

Li, Huarong; Shu, Yuanjie; Gao, Shijie; Chen, Ling; Ma, Qing; Ju, Xuehai

2013-11-01

2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20) is a high-energy nitramine explosive with high mechanical sensitivity. 2,4,6-trinitrotoluene (TNT) is insensitive but by no means a high performance explosive. To reveal the significant importance and smart-material functionality of the energetic-energetic co-crystals, the stability, mechanical and explosive properties TNT/CL-20 co-crystal, TNT crystal and CL-20 crystal were studied. Non-hydrogen bonded non-covalent interactions govern the structures of energetic-energetic co-crystals. However, it is very difficult to accurately calculate the non-covalent intermolecular interaction energies. In this paper, the local conformation and the intricate non-covalent interactions were effectively mapped and analyzed from the electron density (ρ) and its derivatives. The results show that the two components TNT and CL-20 are connected mainly by nitro-aromatic interactions, and nitro-nitro interactions. The steric interactions in TNT/CL-20 could not be confronted with the attractive interactions. Moreover, the scatter graph of TNT crystal reveals the reason why TNT is brittle. The detailed electrostatic potential analysis predicted that the detonation velocities (D) and impact sensitivity for the compounds both increase in the sequence of CL-20 > TNT/CL-20 co-crystal > TNT. Additionally, TNT/CL-20 co-crystal has better malleability than its pure components. This demonstrates the capacity and the feasibility of realizing explosive smart materials by co-crystallization, even if strong hydrogen bonding schemes are generally lacking in energetic materials.

Crystal methamphetamine use and HIV medical outcomes among HIV-infected men who have sex with men accessing support services in New York.

PubMed

Feldman, Matthew B; Thomas, Jacinthe A; Alexy, Emily R; Irvine, Mary K

2015-02-01

Drug use poses multiple challenges to maintaining physical health among HIV-infected individuals, particularly with regard to disease progression. Few studies, however, have examined the association between the use of crystal methamphetamine ("crystal meth") and HIV disease progression specifically among HIV-infected men who have sex with men (MSM). Understanding this relationship among HIV-infected MSM is particularly critical because of the high rates of crystal meth use reported in the population. Associations between recent crystal meth use and poor HIV medical outcomes (viral load>200 copies/mL, CD4 count <350 cells/mm(3)) were analyzed for 2896 HIV-infected MSM enrolled in Ryan White Part A programs in the greater New York metropolitan area between November 2010 and June 2012. Crystal meth use (reported by 4%) was independently associated with unsuppressed viral load (AOR=1.8, CI=1.1-2.9) in multivariate analyses controlling for sociodemographic characteristics. There was no significant relationship between crystal meth use and low CD4 counts. To date, little research has examined how crystal meth use influences HIV medical outcomes among HIV-infected MSM. This analysis showed a significant independent association between crystal meth use and unsuppressed viral load among MSM in an HIV service population. Future studies should examine biological and psychosocial mediators, moderators and confounders of this relationship to inform intervention development for MSM crystal meth users in HIV care settings. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Non-isothermal Crystallization Kinetics of Mold Fluxes for Casting High-Aluminum Steels

NASA Astrophysics Data System (ADS)

Zhou, Lejun; Li, Huan; Wang, Wanlin; Wu, Zhaoyang; Yu, Jie; Xie, Senlin

2017-12-01

This paper investigates the crystallization behavior of CaO-SiO2- and CaO-Al2O3-based mold fluxes for casting high-aluminum steels using single hot thermocouple technology, developed kinetic models, and scanning electron microscope. The results showed that the crystallization ability of the typical CaO-SiO2-based Flux A (CaO/SiO2 0.62, Al2O3 2 mass pct) is weaker than that of CaO-Al2O3-based Flux B (CaO/SiO2 4.11, Al2O3 31.9 mass pct) because of its higher initial crystallization temperature. The crystallization kinetics of Flux A was "surface nucleation and growth, interface reaction control" in the overall non-isothermal crystallization process, whereas that of Flux B was "constant nucleation rate, 1-dimensional growth, diffusion control, in the primary crystallization stage, and then transformed into constant nucleation rate, 3-dimensional growth, interface reaction control in the secondary crystallization stage." The energy dispersive spectroscopy results for Flux B suggested that the variations in the crystallization kinetics for Flux B are due to different crystals precipitating in the primary (BaCa2Al8O15) and secondary (CaAl2O4) crystallization periods during the non-isothermal crystallization process.

Ultrasonication as a potential tool to predict solute crystallization in freeze-concentrates.

PubMed

Ragoonanan, Vishard; Suryanarayanan, Raj

2014-06-01

We hypothesize that ultrasonication can accelerate solute crystallization in freeze-concentrates. Our objective is to demonstrate ultrasonication as a potential predictive tool for evaluating physical stability of excipients in frozen solutions. The crystallization tendencies of lyoprotectants (trehalose, sucrose), carboxylic acid buffers (citric, tartaric, malic, and acetic) and an amino acid buffer (histidine HCl) were studied. Aqueous solutions of buffers, lyoprotectants and mixtures of the two were cooled from room temperature to -20°C and sonicated to induce solute crystallization. The crystallized phases were identified by X-ray diffractometry (laboratory or synchrotron source). Sonication accelerated crystallization of trehalose dihydrate in frozen trehalose solutions. Sonication also enhanced solute crystallization in tartaric (200 mM; pH 5), citric (200 mM pH 4) and malic (200 mM; pH 4) acid buffers. At lower buffer concentrations, longer annealing times following sonication were required to facilitate solute crystallization. The time for crystallization of histidine HCl progressively increased as a function of sucrose concentration. The insonation period required to effect crystallization also increased with sucrose concentration. Sonication can substantially accelerate solute crystallization in the freeze-concentrate. Ultrasonication may be useful in assessing the crystallization tendency of formulation constituents used in long term frozen storage and freeze-drying.

New shield for gamma-ray spectrometry

NASA Technical Reports Server (NTRS)

Brar, S. S.; Gustafson, P. F.; Nelson, D. M.

1969-01-01

Gamma-ray shield that can be evacuated, refilled with a clean gas, and pressurized for exclusion of airborne radioactive contaminants effectively lowers background noise. Under working conditions, repeated evacuation and filling procedures have not adversely affected the sensitivity and resolution of the crystal detector.

Efficient dual-wavelength laser at 946 and 1064 nm with compactly combined Nd:YAG and Nd:YVO4 crystals

NASA Astrophysics Data System (ADS)

Cho, C. Y.; Chang, C. C.; Chen, Y. F.

2013-04-01

We originally employ a compact combination of a Nd:YAG crystal and a Nd:YVO4 crystal to develop an efficient dual-wavelength laser operating at 946 and 1064 nm. We exploit a short Nd:YAG crystal to generate 946 nm laser by reducing the reabsorption loss and a follow-up Nd:YVO4 crystal to generate a 1064 nm laser by absorbing the residual pump light. The output power ratio between the 946 and 1064 nm emissions can be flexibly adjusted from 0.3 to 0.9 by varying the separation between the two output couplers. At an incident pump power of 17 W, the total output power is generally higher than 5.2 W, with an overall optical-to-optical efficiency greater than 30%.

The Use of Atomic-Force Microscopy for Studying the Crystallization Process of Amorphous Alloys

NASA Astrophysics Data System (ADS)

Elmanov, G. N.; Ivanitskaya, E. A.; Dzhumaev, P. S.; Skrytniy, V. I.

The crystallization process of amorphous alloys is accompanied by the volume changes as a result of structural phase transitions. This leads to changes in the surface topography, which was studied by atomic force microscopy (AFM). The changes of the surface topography, structure and phase composition during multistage crystallization process of the metallic glasses with composition Ni71,5Cr6,8Fe2,7B11,9Si7,1 and Ni63,4Cr7,4Fe4,3Mn0,8B15,6Si8,5 (AWS BNi2) has been investigated. The obtained results on changing of the surface topography in crystallization process are in good agreement with the data of X-ray diffraction analysis (XRD). The nature of redistribution of some alloy components in the crystallization process has been suggested.

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Surface Modification and Nanojunction Fabrication with Molecular Metal Wires

DTIC Science & Technology

2012-12-21

single - crystal X-ray diffraction studies of 2 and 3. Both the single - crystal structural data of 2 and 3 and the spectroscopic/voltammetric data...structure, magnetic properties, and single -molecule conductance of two new trinuclear metal string complexes, [Ni3(dzp)4(NCS)2] (2) and [ Co3 (dzp)4(NCS...modifying the crystallization conditions. The [s- Co3 (dpa)4(Cl)2] contains a symmetrical tricobalt framework with identical Co–Co bond lengths (2.34 Å

Crystal structure of 4,5-dinitro-1 H-imidazole

DOE PAGES

Windler, G. Kenneth; Scott, Brian L.; Tomson, Neil C.; ...

2015-01-01

Here, the title compound, C 3H 2N 4O 4, forms crystals with two molecules in the asymmetric unit which are conformationally similar. With the exception of the O atoms of the nitro groups, the molecules are essentially planar. In the crystal, adjacent molecules are associated by N—H...N hydrogen bonds involving the imidazole N—H donors and N-atom acceptors of the unsaturated nitrogen of neighboring rings, forming layers parallel to (010).

A new type of two-dimensional carbon crystal prepared from 1,3,5-trihydroxybenzene

NASA Astrophysics Data System (ADS)

Du, Qi-Shi; Tang, Pei-Duo; Huang, Hua-Lin; Du, Fang-Li; Huang, Kai; Xie, Neng-Zhong; Long, Si-Yu; Li, Yan-Ming; Qiu, Jie-Shan; Huang, Ri-Bo

2017-01-01

A new two-dimensional (2D) carbon crystal, different from graphene, has been prepared from 1,3,5-trihydroxybenzene, consisting of 4-carbon and 6-carbon rings in 1:1 ratio, named 4-6 carbophene by authors, in which all carbon atoms possess sp2 hybrid orbitals with some distortion, forming an extensive conjugated π-bonding planar structure. The angles between the three σ-bonds of the carbon sp2 orbitals are roughly 120°, 90°, and 150°. Each of the three non-adjacent sides of a 6C-ring is shared with a 4C-ring; and each of the two opposite sides of a 4C-ring is shared with a 6C-ring. Dodecagonal holes with a diameter of approximate 5.8 Å are regularly located throughout the 2D carbon crystal. Even though the bond energies in 4-6 carbophene are weaker than those in the graphene, the new planar crystal is quite stable in ambient conditions. The 4-6 carbophene can be synthetized from 1,3,5-trihydroxybenzene or other benzene derivatives through dehydration and polymerization reactions, and may possess several possible patterns that form a family of 2D carbon crystals. A possible side reaction involving 1,3,5-trihydroxybenzene is also discussed, which may produce a carbon-oxygen two dimensional crystal.

Assessment of growth and spectral properties of Cr3+-doped La0.83Y0.29Sc2.88(BO3)4 crystal

NASA Astrophysics Data System (ADS)

Huang, Yisheng; Sun, Shijia; Lin, Zhoubin; Zhang, Lizhen; Wang, Guofu

2017-10-01

This paper reports the spectral characteristic of Cr3+-doped La0.83Y0.29 Sc2.88 (BO3)4 crystal. Cr3+-doped La0.83Y0.29Sc2.88 (BO3)4 crystal was grown from a flux of Li6B4O9 by the top seeded Solution growth method. Cr3+:La0.83Y0.29 Sc2.88 (BO3)4 crystal exhibits broad absorption and emission bands of Cr3+ ions. The absorption cross-section σa is 3.38 × 10-20 cm2 at 467 nm and 4.40 × 10-20 cm2 at 656 nm for E//c, respectively. The emission band with a peak at 906 nm has a full width at half maximum (FWHM) of 188 nm for E//c. The emission cross-section σe at 906 nm is 2.35 × 10-20 cm2 for E//c axis and 2.03 × 10-20 cm2 for E⊥c axis. The fluorescence lifetime of 4T2 → 4A2 transition is 37.7 μs. The investigated result indicates that it may be considered as a potential CW tunable laser crystal material.

Measurement of intrinsic radioactive backgrounds from the 137Cs and U/Th chains in CsI(Tl) crystals

NASA Astrophysics Data System (ADS)

Liu, Shu-Kui; Yue, Qian; Lin, Shin-Ted; Li, Yuan-Jing; Tang, Chang-Jian; Wong Tsz-King, Henry; Xing, Hao-Yang; Yang, Chao-Wen; Zhao, Wei; Zhu, Jing-Jun

2015-04-01

The inorganic CsI(Tl) crystal scintillator is a candidate anti-compton detector for the China Dark matter Experiment. Studying the intrinsic radiopurity of the CsI(Tl) crystal is an issue of major importance. The timing, energy and spatial correlations, as well as the capability of pulse shape discrimination provide powerful methods for the measurement of intrinsic radiopurities. The experimental design, detector performance and event-selection algorithms are described. A total of 359×3 kg-days data from three prototypes of CsI(Tl) crystals were taken at China Jinping Underground Laboratory (CJPL), which offers a good shielding environment. The contamination levels of internal isotopes from 137Cs, 232Th and 238U series, as well as the upper bounds of 235U series are reported. Identification of the whole α peaks from U/Th decay chains and derivation of those corresponding quenching factors are achieved. Supported by National Natural Science Foundation of China (11275107, 11175099)

Ultrafast state detection and 2D ion crystals in a Paul trap

NASA Astrophysics Data System (ADS)

Ip, Michael; Ransford, Anthony; Campbell, Wesley

2016-05-01

Projective readout of quantum information stored in atomic qubits typically uses state-dependent CW laser-induced fluorescence. This method requires an often sophisticated imaging system to spatially filter out the background CW laser light. We present an alternative approach that instead uses simple pulse sequences from a mode-locked laser to affect the same state-dependent excitations in less than 1 ns. The resulting atomic fluorescence occurs in the dark, allowing the placement of non-imaging detectors right next to the atom to improve the qubit state detection efficiency and speed. We also study 2D Coulomb crystals of atomic ions in an oblate Paul trap. We find that crystals with hundreds of ions can be held in the trap, potentially offering an alternative to the use of Penning traps for the quantum simulation of 2D lattice spin models. We discuss the classical physics of these crystals and the metastable states that are supported in 2D. This work is supported by the US Army Research Office.

Correlated Protein Motion Measurements of Dihydrofolate Reductase Crystals

NASA Astrophysics Data System (ADS)

Xu, Mengyang; Niessen, Katherine; Pace, James; Cody, Vivian; Markelz, Andrea

2014-03-01

We report the first direct measurements of the long range structural vibrational modes in dihydrofolate reductase (DHFR). DHFR is a universal housekeeping enzyme that catalyzes the reduction of 7,8-dihydrofolate to 5,6,7,8-tetra-hydrofolate, with the aid of coenzyme nicotinamide adenine dinucleotide phosphate (NADPH). This crucial enzymatic role as the target for anti-cancer [methotrexate (MTX)], and other clinically useful drugs, has made DHFR a long-standing target of enzymological studies. The terahertz (THz) frequency range (5-100 cm-1), corresponds to global correlated protein motions. In our lab we have developed Crystal Anisotropy Terahertz Microscopy (CATM), which directly measures these large scale intra-molecular protein vibrations, by removing the relaxational background of the solvent and residue side chain librational motions. We demonstrate narrowband features in the anisotropic absorbance for mouse DHFR with the ligand binding of NADPH and MTX single crystals as well as Escherichia coli DHFR with the ligand binding of NADPH and MTX single crystals. This work is supported by NSF grant MRI2 grant DBI2959989.

Shear-induced partial translational ordering of a colloidal solid

NASA Astrophysics Data System (ADS)

Ackerson, B. J.; Clark, N. A.

1984-08-01

Highly charged submicrometer plastic spheres suspended in water at low ionic strength will order spontaneously into bcc crystals or polycrystals. A simple linear shear orients and disorders these crystals by forcing (110) planes to stack normal to the shear gradient and to slide relative to each other with a <111> direction parallel to the solvent flow. In this paper we analyze in detail the disordering and flow processes occurring beyond the intrinsic elastic limit of the bcc crystal. We are led to a model in which the flow of a colloidal crystal is interpreted as a fundamentally different process from that found in atomic crystals. In the colloidal crystal the coupling of particle motion to the background fluid forces a homogeneous flow, where every layer is in motion relative to its neighboring layers. In contrast, the plastic flow in an atomic solid is defect mediated flow. At the lowest applied stress, the local bcc order in the colloidal crystal exhibits shear strains both parallel and perpendicular to the direction of the applied stress. The magnitude of these deformations is estimated using the configurational energy for bcc and distorted bcc crystals, assuming a screened Coulomb pair interaction between colloidal particles. As the applied stress is increased, the intrinsic elastic limit of the crystal is exceeded and the crystal begins to flow with adjacent layers executing an oscillatory path governed by the balance of viscous and screened Coulomb forces. The path takes the structure from the bcc1 and bcc2 twins observed at zero shear to a distorted two-dimensional hcp structure at moderate shear rates, with a loss of interlayer registration as the shear is increased. This theoretical model is consistent with other experimental observations, as well.

Suppression of Raman electron spin relaxation of radicals in crystals. Comparison of Cu2+ and free radical relaxation in triglycine sulfate and Tutton salt single crystals.

PubMed

Hoffmann, S K; Goslar, J; Lijewski, S

2011-08-31

Electron spin-lattice relaxation was measured by the electron spin echo method in a broad temperature range above 4.2 K for Cu(2+) ions and free radicals produced by ionizing radiation in triglycine sulfate (TGS) and Tutton salt (NH4)(2)Zn(SO4)2 ⋅ 6H2O crystals. Localization of the paramagnetic centres in the crystal unit cells was determined from continuous wave electron paramagnetic resonance spectra. Various spin relaxation processes and mechanisms are outlined. Cu(2+) ions relax fast via two-phonon Raman processes in both crystals involving the whole phonon spectrum of the host lattice. This relaxation is slightly slower for TGS where Cu(2+) ions are in the interstitial position. The ordinary Raman processes do not contribute to the radical relaxation which relaxes via the local phonon mode. The local mode lies within the acoustic phonon band for radicals in TGS but within the optical phonon range in (NH4)(2)Zn(SO4)2 ⋅ 6H2O. In the latter the cross-relaxation was considered. A lack of phonons around the radical molecules suggested a local crystal amorphisation produced by x- or γ-rays.

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

NASA Technical Reports Server (NTRS)

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

2003-01-01

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

Growth Temperature Dependence of Morphology of GaN Single Crystals in the Na-Li-Ca Flux Method

NASA Astrophysics Data System (ADS)

Wu, Xi; Hao, Hangfei; Li, Zhenrong; Fan, Shiji; Xu, Zhuo

2018-02-01

In this paper, the effect of growth temperature on the morphology and transparency of the GaN crystals obtained by the Li-Ca-added Na Flux method was studied. Addition of Li-Ca was attempted to control the growth habit and further improve transparency of GaN crystals. The samples with wurtzite structure of GaN were confirmed by the x-ray powder diffraction analysis. GaN single crystal with maximum size of about 6 mm was grown at 750°C. As the growth temperature was increased from 700°C to 850°C, the morphology of the crystals changed from pyramid to prism, and their surfaces became smooth. It was found that high growth temperature was beneficial to obtain a transparent crystal, but the evaporation of sodium would suppress its further growth. The E 2 (high) mode in the Raman spectra was at 568 cm-1, and the full-width at half-maximum values of this peak for the crystals obtained at 700°C, 750°C, 800°C, and 850°C were 7.5 cm-1, 10.3 cm-1, 4.4 cm-1, and 4.0 cm-1, respectively. It indicates that all the crystals are stress free and the transparent crystal grown at high temperature has high structural quality or low impurity concentrations.

Synthesis, growth, structural and optical studies of organic nonlinear optical material--piperazine-1,4-diium bis 2,4,6-trinitrophenolate.

PubMed

Suguna, S; Anbuselvi, D; Jayaraman, D; Nagaraja, K S; Jeyaraj, B

2014-11-11

Piperazine-1,4-diium bis 2,4,6-trinitrophenolate is one of the useful organic materials with nonlinear optical (NLO) and pharmaceutical applications. The material was grown by slow evaporation solution growth method at room temperature. The crystal system and lattice parameters were identified by single crystal XRD analysis. The grown material crystallizes in monoclinic system with P21/n space group. The main functional groups NH2, NO2, CN, CC, and phenolic 'O' atom were identified using FTIR analysis. The protons and carbons of grown crystal with various chemical environments were studied by 1H and 13C NMR spectroscopy to confirm the molecular structure. The optical properties of the crystal were studied by UV-vis-NIR spectroscopy and the transmission 100% range starts from 532 nm onwards. The optical band gap was measured as 2.63 eV from the plot of (αhν)2 versus hν. The thermal stability was detected at 304.1°C using TG-DTA analysis. The dielectric studies of the sample were carried out at different temperatures in the frequency range from 50 Hz to 5 MHz to establish the dielectric nature of the crystal. Photoconductivity measurements were carried out on the grown crystal. The Second Harmonic Generation (SHG) of the crystal was tested to confirm the nonlinear optical property. Copyright © 2014 Elsevier B.V. All rights reserved.

Modeling surface backgrounds from radon progeny plate-out

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

Perumpilly, G.; Guiseppe, V. E.; Snyder, N.

2013-08-08

The next generation low-background detectors operating deep underground aim for unprecedented low levels of radioactive backgrounds. The surface deposition and subsequent implantation of radon progeny in detector materials will be a source of energetic background events. We investigate Monte Carlo and model-based simulations to understand the surface implantation profile of radon progeny. Depending on the material and region of interest of a rare event search, these partial energy depositions can be problematic. Motivated by the use of Ge crystals for the detection of neutrinoless double-beta decay, we wish to understand the detector response of surface backgrounds from radon progeny. Wemore » look at the simulation of surface decays using a validated implantation distribution based on nuclear recoils and a realistic surface texture. Results of the simulations and measured α spectra are presented.« less

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

Modeling the intermolecular interactions: molecular structure of N-3-hydroxyphenyl-4-methoxybenzamide.

PubMed

Karabulut, Sedat; Namli, Hilmi; Kurtaran, Raif; Yildirim, Leyla Tatar; Leszczynski, Jerzy

2014-03-01

The title compound, N-3-hydroxyphenyl-4-methoxybenzamide (3) was prepared by the acylation reaction of 3-aminophenol (1) and 4-metoxybenzoylchloride (2) in THF and characterized by ¹H NMR, ¹³C NMR and elemental analysis. Molecular structure of the crystal was determined by single crystal X-ray diffraction and DFT calculations. 3 crystallizes in monoclinic P2₁/c space group. The influence of intermolecular interactions (dimerization and crystal packing) on molecular geometry has been evaluated by calculations performed for three different models; monomer (3), dimer (4) and dimer with added unit cell contacts (5). Molecular structure of 3, 4 and 5 was optimized by applying B3LYP method with 6-31G+(d,p) basis set in gas phase and compared with X-ray crystallographic data including bond lengths, bond angles and selected dihedral angles. It has been concluded that although the crystal packing and dimerization have a minor effect on bond lengths and angles, however, these interactions are important for the dihedral angles and the rotational conformation of aromatic rings. Copyright © 2013 Elsevier Inc. All rights reserved.

Evaporative crystallization of salts from Electrodialysis concentrated brine at atmospheric and subatmospheric pressures

NASA Astrophysics Data System (ADS)

Wang, Dong; Du, Wei; Cheng, Penggao; Tang, Na; Wang, Xuekui

2018-02-01

A large amount of concentrated brine was produced as by-product during the process of the electrodialysis seawater desalination. In this study, the crystallization sequences of different salts from the brine through evaporative crystallization at both atmospheric and subatmospheric pressures were investigated in detail. The profile of the boiling temperature with density and the relationship between the boiling temperature and the pressure were recorded. The combination of Powder X-Ray Diffraction and the polarizing microscope was employed to identify the salts in the solid form. It can be inferred that NaCl crystallized out firstly and then MgSO4·6H2O and CaSO4 precipitate in order at both atmospheric and subatmospheric pressures, and it should be noticed that CaSO4 crystallized as anhydrate at 70°C and 90°C while as dihydrate at 50°C. At the end of all the experiments the precipitation rates of CaSO4 and NaCl have reached to more than 95% while MgSO4 only reached to about 60%.

The role of hydrogen bonds in the crystals of 2-amino-4-methyl-5-nitropyridinium trifluoroacetate monohydrate and 4-hydroxybenzenesulfonate - X-ray and spectroscopic studies.

PubMed

Bryndal, I; Marchewka, M; Wandas, M; Sąsiadek, W; Lorenc, J; Lis, T; Dymińska, L; Kucharska, E; Hanuza, J

2014-04-05

Two new organic-organic salts, 2-amino-4-methyl-5-nitropyridinium trifluoroacetate monohydrate (AMNP-TFA), and 2-amino-4-methyl-5-nitropyridinium 4-hydroxybenzenesulfonate (AMNP-HBS), were obtained and characterized by means of FT-IR, FT-Raman and single crystal X-ray crystallography. In the former crystal, the cations, anions and water molecules are linked into layers by three types of hydrogen bonds, NPH⋯O, NAH⋯O and OH⋯O. These layers are connected by weaker CH⋯O hydrogen bonds. In the latter crystal, the cations and anions form one-dimensional structure through a number of hydrogen-bonding interactions involving the OH, NH(+) and NH2 groups as donors. In this case the NPH⋯O and NAH⋯O hydrogen bonds are formed. The combination of interactions between cations and anions results in the formation of columns. Additionally, there are π-π stacking interactions between the columns. The obtained X-ray structural data are related to the vibrational spectra of the studied crystals. Copyright © 2013 Elsevier B.V. All rights reserved.

Crystal structures of 4-meth-oxy-N-(4-methyl-phenyl)benzene-sulfonamide and N-(4-fluoro-phenyl)-4-meth-oxy-benzene-sulfonamide.

PubMed

Rodrigues, Vinola Z; Preema, C P; Naveen, S; Lokanath, N K; Suchetan, P A

2015-11-01

Crystal structures of two N-(ar-yl)aryl-sulfonamides, namely, 4-meth-oxy-N-(4-methyl-phen-yl)benzene-sulfonamide, C14H15NO3S, (I), and N-(4-fluoro-phen-yl)-4-meth-oxy-benzene-sulfonamide, C13H12FNO3S, (II), were determined and analyzed. In (I), the benzene-sulfonamide ring is disordered over two orientations, in a 0.516 (7):0.484 (7) ratio, which are inclined to each other at 28.0 (1)°. In (I), the major component of the sulfonyl benzene ring and the aniline ring form a dihedral angle of 63.36 (19)°, while in (II), the planes of the two benzene rings form a dihedral angle of 44.26 (13)°. In the crystal structure of (I), N-H⋯O hydrogen bonds form infinite C(4) chains extended in [010], and inter-molecular C-H⋯πar-yl inter-actions link these chains into layers parallel to the ab plane. The crystal structure of (II) features N-H⋯O hydrogen bonds forming infinite one dimensional C(4) chains along [001]. Further, a pair of C-H⋯O inter-molecular inter-actions consolidate the crystal packing of (II) into a three-dimensional supra-molecular architecture.

Structural and computational study of 1,2,4-triazolin-5-thione derivative and its DMSO solvate

NASA Astrophysics Data System (ADS)

Dybała, Izabela; Wawrzycka-Gorczyca, Irena; Struga, Marta

2017-11-01

The solid state structure of 3-(4-phenyl-5-oxo-1,2,4-triazolin-1-ylmethyl)-4-cyclohexyl-1,2,4-triazolin-5-thione (1) was characterized by FT-IR and X-ray diffraction experiment. Additionally, molecular and crystal structure of its DMSO solvate (1DMSO) has been determined by X-ray diffraction method. The influence of DMSO molecules incorporation to the crystal lattice on geometry of triazolin-5-thione derivative molecule and crystal packing was analyzed. Non-covalent bonds within the crystals are additionally visualized by determination of Hirshfeld surfaces. According to results of conformational analysis in gas, molecule of triazolin-5-thione derivative adopts the lowest energy conformation in 1DMSO crystal. The crystal structure of 1 and 1DMSO were compared with previously described structurally similar compounds, in which the cyclohexyl substituent was replaced by aromatic one (phenyl/methoxyphenyl). Very interesting differences in molecules association were found by comparing the crystal structures of 1 and 1DMSO with their, mentioned above, aromatic derivatives. Interesting properties of triazolin-5-thione derivatives are connected with their π-electron delocalization effects, thus aromaticity of heterocyclic fragments has been investigated by means of the HOMA index. Comparison of aromaticity calculations results with association tendency of molecules shows that triazolin-5-one fragments reach higher aromaticity when nitrogen atom from this moiety acts as a donor in strong Nsbnd H⋯N hydrogen bonds.

Effect of cationic substitution on the double-well hydrogen-bond potential in [K1-x(NH4)x]3H(SO4)2 proton conductors: a single-crystal neutron diffraction study.

PubMed

Choudhury, R R; Chitra, R; Selezneva, E V; Makarova, I P

2017-10-01

The structure of the mixed crystal [K 1-x (NH 4 ) x ] 3 H(SO 4 ) 2 as obtained from single-crystal neutron diffraction is compared with the previously reported room-temperature neutron structure of crystalline K 3 H(SO 4 ) 2 . The two structures are very similar, as indicated by the high value of their isostructurality index (94.8%). It was found that the replacement of even a small amount (3%) of K + with NH 4 + has a significant influence on the short strong hydrogen bond connecting the two SO 4 2- ions. Earlier optical measurements had revealed that the kinetics of the superionic transition in the solid solution [K 1-x (NH 4 ) x ] 3 H(SO 4 ) 2 are much faster than in K 3 H(SO 4 ) 2 ; this reported difference in the kinetics of the superionic phase transition in this class of crystal is explained on the basis of the difference in strength of the hydrogen-bond interactions in the two structures.

Bis (3-methoxy-4-hydroxybenzaldehyde-2,4,6-trinitrophenol) organic cocrystal: Synthesis and physico-chemical properties

NASA Astrophysics Data System (ADS)

Sudharsana, N.; Krishnakumar, V.; Nagalakshmi, R.

2016-10-01

A 3-methoxy-4-hydroxybenzaldehyde-2,4,6-trinitrophenol (mhba-tnp) cocrystal was grown by the slow evaporation solution growth technique using ethanol as a solvent. As-grown crystals were characterized by single crystal X-ray diffraction (XRD) study and crystallized with a centrosymmetric space group. Optical properties of the grown crystal have been studied by Ultraviolet-Visible (UV-Vis) absorption spectra in the range from 200 to 800nm and the band gap energy of the crystal was obtained as 2.8eV. Fourier transform infrared (FTIR) and micro Raman spectral analyses have been carried out to confirm the functional groups present in the title compound. Differential scanning calorimetry (DSC) and polarized light thermomicroscopy (PLTM) analyses were carried out to find the melting point. In addition, the optimized geometric parameters and the molecular orbitals were calculated using density functional theory (DFT) with the help of the Gaussian 03W software.

Theoretical investigation of the formation of basal plane stacking faults in heavily nitrogen-doped 4H-SiC crystals

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

Taniguchi, Chisato; Ichimura, Aiko; Ohtani, Noboru, E-mail: ohtani.noboru@kwansei.ac.jp

The formation of basal plane stacking faults in heavily nitrogen-doped 4H-SiC crystals was theoretically investigated. A novel theoretical model based on the so-called quantum well action mechanism was proposed; the model considers several factors, which were overlooked in a previously proposed model, and provides a detailed explanation of the annealing-induced formation of double layer Shockley-type stacking faults in heavily nitrogen-doped 4H-SiC crystals. We further revised the model to consider the carrier distribution in the depletion regions adjacent to the stacking fault and successfully explained the shrinkage of stacking faults during annealing at even higher temperatures. The model also succeeded inmore » accounting for the aluminum co-doping effect in heavily nitrogen-doped 4H-SiC crystals, in that the stacking fault formation is suppressed when aluminum acceptors are co-doped in the crystals.« less

Crystal phase-based epitaxial growth of hybrid noble metal nanostructures on 4H/fcc Au nanowires

NASA Astrophysics Data System (ADS)

Lu, Qipeng; Wang, An-Liang; Gong, Yue; Hao, Wei; Cheng, Hongfei; Chen, Junze; Li, Bing; Yang, Nailiang; Niu, Wenxin; Wang, Jie; Yu, Yifu; Zhang, Xiao; Chen, Ye; Fan, Zhanxi; Wu, Xue-Jun; Chen, Jinping; Luo, Jun; Li, Shuzhou; Gu, Lin; Zhang, Hua

2018-03-01

Crystal-phase engineering offers opportunities for the rational design and synthesis of noble metal nanomaterials with unusual crystal phases that normally do not exist in bulk materials. However, it remains a challenge to use these materials as seeds to construct heterometallic nanostructures with desired crystal phases and morphologies for promising applications such as catalysis. Here, we report a strategy for the synthesis of binary and ternary hybrid noble metal nanostructures. Our synthesized crystal-phase heterostructured 4H/fcc Au nanowires enable the epitaxial growth of Ru nanorods on the 4H phase and fcc-twin boundary in Au nanowires, resulting in hybrid Au-Ru nanowires. Moreover, the method can be extended to the epitaxial growth of Rh, Ru-Rh and Ru-Pt nanorods on the 4H/fcc Au nanowires to form unique hybrid nanowires. Importantly, the Au-Ru hybrid nanowires with tunable compositions exhibit excellent electrocatalytic performance towards the hydrogen evolution reaction in alkaline media.

Towards Protein Crystallization as a Process Step in Downstream Processing of Therapeutic Antibodies: Screening and Optimization at Microbatch Scale

PubMed Central

Zang, Yuguo; Kammerer, Bernd; Eisenkolb, Maike; Lohr, Katrin; Kiefer, Hans

2011-01-01

Crystallization conditions of an intact monoclonal IgG4 (immunoglobulin G, subclass 4) antibody were established in vapor diffusion mode by sparse matrix screening and subsequent optimization. The procedure was transferred to microbatch conditions and a phase diagram was built showing surprisingly low solubility of the antibody at equilibrium. With up-scaling to process scale in mind, purification efficiency of the crystallization step was investigated. Added model protein contaminants were excluded from the crystals to more than 95%. No measurable loss of Fc-binding activity was observed in the crystallized and redissolved antibody. Conditions could be adapted to crystallize the antibody directly from concentrated and diafiltrated cell culture supernatant, showing purification efficiency similar to that of Protein A chromatography. We conclude that crystallization has the potential to be included in downstream processing as a low-cost purification or formulation step. PMID:21966480

Crystal structure and vibrational spectra of melaminium arsenate

NASA Astrophysics Data System (ADS)

Anbalagan, G.; Marchewka, M. K.; Pawlus, K.; Kanagathara, N.

2015-01-01

The crystals of the new melaminium arsenate (MAS) [C3H7N6+ṡH2AsO4-] were obtained by the slow evaporation of an aqueous solution at room temperature. Single crystal X-ray diffraction analysis reveals that the crystal belongs to triclinic system with centro symmetric space group P-1. The crystals are built up from single protonated melaminium residues and single dissociated arsenate H2AsO4- anions. The protonated melaminium ring is almost planar. A combination of ionic and donor-acceptor hydrogen-bond interactions linking together the melaminium and arsenate residues forms a three-dimensional network. Vibrational spectroscopic analysis is reported on the basis of FT-IR and FT-Raman spectra recorded at room temperature. Hydrogen bonded network present in the crystal gives notable vibrational effect. DSC has also been performed for the crystal shows no phase transition in the studied temperature range (113-293 K).

The cluster compound In{sub 4}Ti{sub 1.5}Mo{sub 0.5}Mo{sub 14}O{sub 26} containing Mo{sub 14} clusters and the new mono- and bi-capped trioctahedral Mo{sub 15} and Mo{sub 16} clusters: Synthesis, crystal structure, and electrical and magnetic properties

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

Gall, Philippe; Guizouarn, Thierry; Gougeon, Patrick, E-mail: Patrick.Gougeon@univ-rennes1.fr

2015-07-15

Single crystals of the new quaternary compound In{sub 4}Ti{sub 1.5}Mo{sub 0.5}Mo{sub 14}O{sub 26} were obtained by solid state reaction. The crystal structure was determined by single-crystal X-ray diffraction. In{sub 4}Ti{sub 1.5}Mo{sub 0.5}Mo{sub 14}O{sub 26} crystallizes in the orthorhombic space group Pbca with unit-cell parameters a=9.4432(14) Å, b=11.4828(12) Å, c=20.299(4) Å and Z=4. Full-matrix least-squares refinement on F{sup 2} using 3807 independent reflections for 219 refinable parameters resulted in R{sub 1}=0.0259 and wR{sub 2}=0.0591. The crystal structure contains in addition to Mo{sub 14} clusters the first examples of mono- and bi-capped trioctahedral Mo{sub 14} i.e. Mo{sub 15} and Mo{sub 16} clusters.more » The oxygen framework derives from a stacking along the a direction of close-packed layers with sequence (…ABAC…). The Mo–Mo distances range between 2.6938(5) and 2.8420(6) Å and the Mo–O distances between 1.879(5) and 2.250(3) Å, as usually observed in molybdenum oxide clusters. The indium atoms form In{sub 4}{sup 6+} bent chains with In–In distances of 2.6682(5) and 2.6622(8) Å and the Ti atoms are in highly distorted octahedral sites of oxygen atoms with Ti–O distances ranging between 1.865(4) and 2.161(4) Å. Magnetic susceptibility measurements confirm the presence of Ti{sup 4+} cations and the absence of localized moments on the Mo network. Electrical resistivity measurements on a single crystal of In{sub 4}Ti{sub 1.5}Mo{sub 0.5}Mo{sub 14}O{sub 26} show a semimetallic behavior. - Graphical abstract: We present here the synthesis, the crystal structure, and the electrical and magnetic properties of the new compound In{sub 4}Ti{sub 1.5}Mo{sub 0.5}Mo{sub 14}O{sub 26} in which Mo{sub 14} clusters coexist statistically with mono- and bi-capped trioctahedral Mo{sub 14} that is Mo{sub 15} and Mo{sub 16} clusters. - Highlights: • Single crystals of In{sub 4}Ti{sub 1.5}Mo{sub 0.5}Mo{sub 14}O{sub 26} were obtained by solid state reaction. • The crystal structure contains Mo{sub 14}, Mo{sub 15} and Mo{sub 16} clusters. • The indium atoms form In{sub 4}{sup 6+} bent chains. • Poorly metallic behavior. • Absence of localized moments on the Mo network as well as on the Ti atoms.« less

Investigation the influences of B2O3 and R2O on the structure and crystallization behaviors of CaO-Al2O3 based F-free mold flux

NASA Astrophysics Data System (ADS)

Li, Jiangling; Kong, Bowen; Gao, Xiangyu; Liu, Qingcai; Shu, Qifeng; Chou, Kuochih

2018-04-01

The influences of B2O3 and R2O on the structure and crystallization of CaO-Al2O3 based F-free mold flux were investigated by Raman Spectroscopy and Differential Scanning Calorimetry Technique, respectively, for developing a new type of F-free mold flux. The results of structural investigations showed that B3+ is mainly in the form of [BO3]. And [BO3] appears to form BIII-O-Al linkage which will produce a positive effect on forming [AlO4] network. The number of bridging oxygen and the degree of polymerization of [AlO4] network structure for CaO-Al2O3 system were also increased with the increasing of B2O3. On the contrary, with the addition of R2O into CaO-Al2O3-B2O3 system, the number of bridging oxygen and the degree of polymerization of [AlO4] network were decreased. DSC results showed that the crystallization process became more sluggish with the increase of B2O3, which indicated that the crystallization ability was weakened. While the quenched mold fluxes crystallized more rapidly when introducing R2O. In other word, the crystallization rates of CaO-Al2O3 based slags were accelerated by the introduction of R2O. The liquidus temperature and crystallization temperature were decreased with the increasing amount of B2O3 or by addition of R2O into CaO-Al2O3 system. Only one kind of crystal was precipitated in 8% B2O3 and %R2O-containing samples, which was CaAl2O4 identified by SEM-EDS. When the content of B2O3 increased from 8% to 16%, Ca3B2O6 is clearly observed, demonstrating that the crystallization ability of Ca3B2O6 is enhanced by the increasing concentration of B2O3 in mold flux. The Ca/Al ratio of the generated calcium aluminate has been altered from 1:2 to 1:4 with the increasing of B2O3. The size of CaAl2O4 crystal is gradually increased with the addition of R2O. The crystallization ability of CaAl2O4 is promoted by R2O.

Radiopaque Strontium Fluoroapatite Glass-Ceramics.

PubMed

Höland, Wolfram; Schweiger, Marcel; Dittmer, Marc; Ritzberger, Christian

2015-01-01

The controlled precipitation of strontium fluoroapatite crystals was studied in four base glass compositions derived from the SiO2-Al2O3-Y2O3-SrO-Na2O-K2O/Rb2O/Cs2O-P2O5-F system. The crystal phase formation of these glasses and the main properties of the glass-ceramics, such as thermal and optical properties and radiopacity were compared with a fifth, a reference glass-ceramic. The reference glass-ceramic was characterized as Ca-fluoroapatite glass-ceramic. The four strontium fluoroapatite glass-ceramics showed the following crystal phases: (a) Sr5(PO4)3F - leucite, KAlSi2O6, (b) Sr5(PO4)3F - leucite, KAlSi2O6, and nano-sized NaSrPO4, (c) Sr5(PO4)3F - pollucite, CsAlSi2O6, and nano-sized NaSrPO4, and (d) Sr5(PO4)3F - Rb-leucite, RbAlSi2O6, and nano-sized NaSrPO4. The proof of crystal phase formation was possible by X-ray diffraction. The microstructures, which were studied using scanning electron microscopy, demonstrated a uniform distribution of the crystals in the glass matrix. The Sr-fluoroapatites were precipitated based on an internal crystallization process, and the crystals demonstrated a needle-like morphology. The study of the crystal growth of needle-like Sr-fluoroapatites gave a clear evidence of an Ostwald ripening mechanism. The formation of leucite, pollucite, and Rb-leucite was based on a surface crystallization mechanism. Therefore, a twofold crystallization mechanism was successfully applied to develop these types of glass-ceramics. The main focus of this study was the controlled development of glass-ceramics exhibiting high radiopacity in comparison to the reference glass-ceramic. This goal could be achieved with all four glass-ceramics with the preferred development of the Sr-fluoroapatite - pollucite-type glass-ceramic. In addition to this main development, it was possible to control the thermal properties. Especially the Rb-leucite containing glass-ceramic showed the highest coefficient of thermal expansion (CTE). These glass-ceramics allow optical properties, especially the translucency and color, to be tailored to the needs of biomaterials for dental applications. The authors conclude that it is possible to use twofold crystallization processes to develop glass-ceramic biomaterials featuring different properties, such as specific radiopacity values, CTEs, and optical characteristics.

Radiopaque Strontium Fluoroapatite Glass-Ceramics

PubMed Central

Höland, Wolfram; Schweiger, Marcel; Dittmer, Marc; Ritzberger, Christian

2015-01-01

The controlled precipitation of strontium fluoroapatite crystals was studied in four base glass compositions derived from the SiO2–Al2O3–Y2O3–SrO–Na2O–K2O/Rb2O/Cs2O–P2O5–F system. The crystal phase formation of these glasses and the main properties of the glass-ceramics, such as thermal and optical properties and radiopacity were compared with a fifth, a reference glass-ceramic. The reference glass-ceramic was characterized as Ca-fluoroapatite glass-ceramic. The four strontium fluoroapatite glass-ceramics showed the following crystal phases: (a) Sr5(PO4)3F – leucite, KAlSi2O6, (b) Sr5(PO4)3F – leucite, KAlSi2O6, and nano-sized NaSrPO4, (c) Sr5(PO4)3F – pollucite, CsAlSi2O6, and nano-sized NaSrPO4, and (d) Sr5(PO4)3F – Rb-leucite, RbAlSi2O6, and nano-sized NaSrPO4. The proof of crystal phase formation was possible by X-ray diffraction. The microstructures, which were studied using scanning electron microscopy, demonstrated a uniform distribution of the crystals in the glass matrix. The Sr-fluoroapatites were precipitated based on an internal crystallization process, and the crystals demonstrated a needle-like morphology. The study of the crystal growth of needle-like Sr-fluoroapatites gave a clear evidence of an Ostwald ripening mechanism. The formation of leucite, pollucite, and Rb-leucite was based on a surface crystallization mechanism. Therefore, a twofold crystallization mechanism was successfully applied to develop these types of glass-ceramics. The main focus of this study was the controlled development of glass-ceramics exhibiting high radiopacity in comparison to the reference glass-ceramic. This goal could be achieved with all four glass-ceramics with the preferred development of the Sr-fluoroapatite – pollucite-type glass-ceramic. In addition to this main development, it was possible to control the thermal properties. Especially the Rb-leucite containing glass-ceramic showed the highest coefficient of thermal expansion (CTE). These glass-ceramics allow optical properties, especially the translucency and color, to be tailored to the needs of biomaterials for dental applications. The authors conclude that it is possible to use twofold crystallization processes to develop glass-ceramic biomaterials featuring different properties, such as specific radiopacity values, CTEs, and optical characteristics. PMID:26528470

Quality inspection of anisotropic scintillating lead tungstate (PbWO 4) crystals through measurement of interferometric fringe pattern parameters

NASA Astrophysics Data System (ADS)

Cocozzella, N.; Lebeau, M.; Majni, G.; Paone, N.; Rinaldi, D.

2001-08-01

Scintillating crystals are widely used as detectors in radiographic systems, computerized axial tomography devices and in calorimeters employed in high-energy physics. This paper results from a project motivated by the development of the CMS calorimeter at CERN, which will make use of a large number of scintillating crystals. In order to prevent crystals from breaking because of internal residual stress, a quality control system based on optic inspection of interference fringe patterns was developed. The principle of measurement procedures was theoretically modelled, and then a dedicated polariscope was designed and built, in order to observe the crystals under induced stresses or to evaluate the residual internal stresses. The results are innovative and open a new perspective for scintillating crystals quality control: the photoelastic constant normal to the optic axis of the lead tungstate crystals (PbWO 4) was measured, and the inspection procedure developed is applicable to mass production, not only to optimize the crystal processing, but also to establish a quality inspection procedure.

Investigations of Q-switching and mode locking in diode-pumped Nd:YVO4 laser with passive saturable absorbers

NASA Astrophysics Data System (ADS)

Kwiatkowski, Jacek; Jabczynski, Jan K.; Zendzian, Waldemar

2005-03-01

The saturable absorbers (Cr4+:YAG, GaAs and LiF crystals for 1064-nm wavelength, V3+:YAG crystals for 1340-nm respectively) were examined as passive Mode Lockers and Q-switches in diode pumped Nd:YVO4 lasers in the Z-type resonators. In each case, partially modulated long trains of QML pulses were observed. As a rule, envelopes with about 1 μs duration and more than 50% depth of modulation were observed. For stabilization of the mode locking trains nonlinear crystals (KTP or LBO) as negative feedback elements were inserted. The fully modulated QML trains for intracavity II harmonic conversion at 670-nm wavelength in V3+:YAG Q-switched Nd:YVO4 laser with LBO crystal were demonstrated.

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.

Spectroscopic, single crystal X-ray, Hirshfeld, in vitro and in silico biological evaluation of a new series of potent thiazole nucleus integrated with pyrazoline scaffolds

NASA Astrophysics Data System (ADS)

Salian, Vinutha V.; Narayana, Badiadka; Sarojini, Balladka K.; Kumar, Madan S.; Nagananda, Govinahalli S.; Byrappa, Kullaiah; Kudva, Avinash K.

2017-03-01

In the present study, the spectroscopic characterization of a new series of substituted thiazole linked pyrazoline scaffolds 4a-l was performed. The formation of 4a-l from the intermediate 3-(4-chlorophenyl)-5-[4-(propan-2-yl)phenyl]-4,5-dihydro-1H-pyrazole-1-carbothioamide 2 and substituted 2-bromo-1-phenylethanone 3a-l was evidenced through the changes in FTIR, 1H NMR, 13C NMR, LCMS data. The X-ray diffraction studies revealed that compound 2 and 4g crystallized in monoclinic crystal system with P21/n space group. Compound 4j crystallized in triclinic system, P1¯ space group with Z = 4. The percentage of intermolecular contacts and distribution of electrostatic potential of molecular crystal structures was resolved by Hirshfeld surface analysis with 2D finger plots and electrostatic potential map. The newly synthesized derivatives were screened for their in vitro antioxidant and antimicrobial activity. The single crystal studies revealed that, for compounds 2, 4g and 4j the isopropyl phenyl ring is positioned at near right angle with the other rings. Due to the lack of planarity of bulkier group substituted to phenyl ring (ring B), all the synthesized molecules showed weak to moderate radical scavenging capacity owing to the destabilization of the radical formed during oxidation. Also, on performing molecular docking studies to explore the interactions of ligand with the target pyrimidine nucleoside hydrolase YbeK with bound ribose complex (PNH, PDB ID-3GHW), disclosed that active compounds emerged for in vitro studies also bound to PNH more efficiently. The compounds with polar group substitution interacted through hydrogen bonding while other molecules with non-covalent interactions.

A chemical bath deposition route to facet-controlled Ag{sub 3}PO{sub 4} thin films with improved visible light photocatalytic activity

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

Gunjakar, Jayavant L.; Jo, Yun Kyung; Kim, In Young

A facile, economic, and reproducible chemical bath deposition (CBD) method is developed for the fabrication of facet-controlled Ag{sub 3}PO{sub 4} thin films with enhanced visible light photocatalytic activity. The fine-control of bath temperature, precursor, complexing agent, substrate, and solution pH is fairly crucial in preparing the facet-selective thin film of Ag{sub 3}PO{sub 4} nanocrystal. The change of precursor from silver nitrate to silver acetate makes possible the tailoring of the crystal shape of Ag{sub 3}PO{sub 4} from cube to rhombic dodecahedron and also the bandgap tuning of the deposited films. The control of [Ag{sup +}]/[phosphate] ratio enables to maximize themore » loading amount of Ag{sub 3}PO{sub 4} crystals per the unit area of the deposited film. All the fabricated Ag{sub 3}PO{sub 4} thin films show high photocatalytic activity for visible light-induced degradation of organic molecules, which can be optimized by tailoring the crystal shape of the deposited crystals. This CBD method is also useful in preparing the facet-controlled hybrid film of Ag{sub 3}PO{sub 4}–ZnO photocatalyst. The present study clearly demonstrates the usefulness of the present CBD method for fabricating facet-controlled thin films of metal oxosalt and its nanohybrid. - Highlights: • The crystal facet of Ag{sub 3}PO{sub 4} films can be tuned by chemical bath deposition. • The crystal shape of Ag{sub 3}PO{sub 4} is tailorable from cube to rhombic dodecahedron. • Facet-tuned Ag{sub 3}PO{sub 4} film shows enhanced visible light photocatalyst activity.« less

XRD, TEM, IR, Raman and NMR Spectroscopy of In Situ Crystallization of Lithium Disilicate Glass

NASA Technical Reports Server (NTRS)

Fuss, T.; Mogus-Milankovic, A.; Ray, C. S.; Lesher, C. E.; Youngman, R.; Day, D. E.

2006-01-01

The structure of a Li2O-2SiO2 (LS2) glass was investigated as a function of pressure and temperature up to 6 GPa and 750 C respectively, using XRD, TEM, IR, Raman and NMR spectroscopy. Glass densified at 6 GPa has an average Si-O-Si bond angle approx.7deg lower than that found in glass processed at 4.5 GPa. At 4.5 GPa, lithium disilicate crystallizes from the glass, while at 6 GPa a new high pressure form of lithium metasilicate crystallizes. The new phase, while having lithium metasilicate crystal symmetry, contains at least 4 different Si sites. NMR results for 6 GPa sample indicate the presence of Q4 species with (Q(sup 4))Si-O-Si(Q(sup 4)) bond angles of approx.157deg. This is the first reported occurrence of Q(sup 4) species with such large bond angles in alumina free alkali silicate glass. No five- or six- coordinated Si are found.

Crystallization kinetics from mixture Na2SO4/glycerol droplets of Na2SO4 by FTIR-ATR

NASA Astrophysics Data System (ADS)

Tan, Dan-Ting; Cai, Chen; Zhang, Yun; Wang, Na; Pang, Shu-Feng; Zhang, Yun-Hong

2016-08-01

The efflorescence of mixed Na2SO4/glycerol aerosols on the ZnSe substrate with various mole ratios (Na2SO4/glycerol = 1:1, 1:2, 1:4) has been studied in the relative humidity (RH) linearly decline process, using a situ Fourier transform infrared attenuated total reflection (FTIR-ATR) technique. The crystal ratio at a given RH can be gained by the absorbance of the band at 1132 cm-1, which shows the incomplete nucleation for mixed Na2SO4/glycerol aerosols and the decreased amount of the droplets crystallized at the lowest RH with the glycerol increase. Using the volume fraction of droplets that have yet to crystallize, the heterogeneous nucleation kinetics has been gained. By the Extended Aerosol Inorganics Model (E-AIM), the nucleation rate as the function of solute saturation degree has been gained for various mixed Na2SO4/glycerol aerosols.

Overexpression, crystallization and preliminary X-­ray crystallographic analysis of erythronate-4-phosphate dehydrogenase from Pseudomonas aeruginosa

PubMed Central

Ha, Jun Yong; Lee, Ji Hyun; Kim, Kyoung Hoon; Kim, Do Jin; Lee, Hyung Ho; Kim, Hye-Kyung; Yoon, Hye-Jin; Suh, Se Won

2006-01-01

The enzyme erythronate-4-phosphate dehydrogenase catalyses the conversion of erythronate-4-phosphate to 3-hydroxy-4-phospho-hydroxy-α-ketobutyrate. It belongs to the d-isomer-specific 2-hydroxyacid dehydrogenase family. It is essential for de novo biosynthesis of vitamin B6 (pyridoxine). Erythronate-4-­phosphate dehydrogenase from Pseudomonas aeruginosa, a homodimeric enzyme consisting of two identical 380-residue subunits, has been overexpressed in Escherichia coli with a C-terminal purification tag and crystallized at 297 K using 0.7 M ammonium dihydrogen phosphate, 0.4 M ammonium tartrate, 0.1 M sodium citrate pH 5.6 and 10 mM cupric chloride. X-ray diffraction data were collected to 2.20 Å from a crystal grown in the presence of NADH. The crystals belong to the orthorhombic space group P212121, with unit-cell parameters a = 84.77, b = 101.28, c = 142.58 Å. A dimeric molecule is present in the asymmetric unit, giving a crystal volume per protein weight (V M) of 3.64 Å3 Da−1 and a solvent content of 66%. PMID:16511285

' Self-organization' processes in proton and deuteron mixtures in open-chain hydrogen bond systems: polarization IR spectra of 4-mercaptopyridine crystals

NASA Astrophysics Data System (ADS)

Flakus, Henryk T.; Tyl, Aleksandra; Jones, Peter G.

2002-01-01

This paper is devoted to IR spectroscopic studies in polarized light of 4-mercaptopyridine (4-MPD) hydrogen-bonded crystals. These studies were preceded by determination of the 4-mercaptopyridine X-ray structure. Polarization spectra of 4-mercaptopyridine crystals were measured in the frequency ranges of νN-H and νN-D bands at room temperature, and also at the temperature of liquid nitrogen, for the two different crystalline faces: ' bc' and ' ac'. When investigating ' residual' νN-H band shapes for crystals that were diluted by deuterium, strong dichroic effects in the spectra were still observed, providing evidence for the existence in the hydrogen bond chains of domains containing exclusively protons or deuterons. This phenomenon proves the existence of a new kind of H/D isotopic effects in open chain hydrogen bond systems, namely ' self-organization' effects. Such effects, however, were not observed for other open chain hydrogen bond systems, e.g. alcohol crystals. Solid-state spectra of 4-mercaptopyridine were quantitatively interpreted, along with the strong polarization and the isotopic effects, when based on the ' strong-coupling' theory for linearly arranged hydrogen bond dimers.

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.

Crystal growth, perfection, linear and nonlinear optical, photoconductivity, dielectric, thermal and laser damage threshold properties of 4-methylimidazolium picrate: an interesting organic crystal for photonic and optoelectronic devices

NASA Astrophysics Data System (ADS)

Rajesh, K.; Arun, A.; Mani, A.; Praveen Kumar, P.

2016-10-01

The 4-methylimidazolium picrate has been synthesized and characterized successfully. Single and powder x-ray diffraction studies were conducted which confirmed the crystal structure, and the value of the strain was calculated. The crystal perfection was determined by a HRXR diffractometer. The transmission spectrum exhibited a better transmittance of the crystal in the entire visible region with a lower cut-off wavelength of 209 nm. The linear absorption value was calculated by the optical limiting method. A birefringence study was also carried out. Second and third order nonlinear optical properties of the crystal were found by second harmonic generation and the z-scan technique. The crystals were also characterized by dielectric measurement and a photoconductivity analyzer to determine the dielectric property and the optical conductivity of the crystal. The laser damage threshold activity of the grown crystal was studied by a Q-switched Nd:YAG laser beam. Thermal studies established that the compound did not undergo a phase transition and was stable up to 240 °C.

Characterization of the electro-optic effect in styrylpyridinium cyanine dye thin-film crystals by an ac modulation method

NASA Astrophysics Data System (ADS)

Yoshimura, Tetsuzo

1987-09-01

The electro-optic effect in styrylpyridinium cyanine dye (SPCD) thin-film crystals is characterized by a newly developed ac modulation method that is effective in characterizing thin-film materials of small area. SPCD thin-film crystals 3-10 μm thick were grown from a methanol solution of SPCD. The crystal shows strong dichroism and anisotropy of refractive index, indicating that molecular dipole moments align along a definite direction (z axis). When an electric field is applied along the z axis, SPCD thin-film crystals show a large figure of merit of electro-optic phase retardation of 6.5×10-10 m/V, which is 5 times as large as in LiNbO3 crystal, 2 times that in 2-methyl-4-nitroaniline (MNA) crystal, and is the largest ever reported in organic solids. The electro-optic coefficient r33 of SPCD crystals is estimated to be approximately 4.3×10-10 m/V, which is 6 times larger than that of an MNA crystal. This value is consistent with that expected from second-harmonic generation measurements.

Crystal growth, polarized spectra, and laser performance of Yb:CaGdAlO4 crystal

NASA Astrophysics Data System (ADS)

Di, J. Q.; Xu, X. D.; Xia, C. T.; Zheng, L. H.; Aka, G.; Yu, H. H.; Sai, Q. L.; Guo, X. Y.; Zhu, L.

2016-04-01

In this paper, the crystal growth, polarized spectra, and laser performance of Yb:CaGdAlO4 crystal were reported. The segregation coefficient of Yb3+ ions was calculated to be 0.47. The cell parameters were determined to be a  =  b  =  0.3658 nm, c  =  1.1985 nm. The peak absorption cross-section was calculated to be 2.65  ×  10-20 cm2 at 979 nm and the peak stimulated emission cross-section was 2.23  ×  10-20 cm2 at 980 nm for the π polarization. The continuous-wave (CW) laser operations of uncoated Yb:CaGdAlO4 crystals with 5  ×  5  ×  3 mm3 in size were demonstrated. A maximum output power of 1.6 W at 1048 nm was obtained with a slope efficiency of 28%. The results show that Yb:CaGdAlO4 crystal is a promising laser medium.

Ultraviolet luninescence of ScPO 4, AlPO 4, and GaPO 4 crystals

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

Trukhin, Anatoly N.; Shmits, Krishjanis; Jansons, Janis L.

2013-08-29

The luminescence of self-trapped excitons (STE) was previously observed and described for the case of tetragonal-symmetry ScPO 4 single crystals in 1996 by Trukhin and Boatner. The subject band in this material is situated in the UV spectral range of ~210 nm or ~5.8 eV. In the present work, we are both expanding this earlier luminescence study and seeking to identify similar luminescence phenomena in other orthophosphate crystals i.e., AlPO 4 and GaPO 4. These efforts have proven to be successful - in spite of the structural differences between these materials and ScPO 4. Specifically we have found that formore » AlPO 4 and GaPO 4, in addition to an -quartz-like STE, there is a UV luminescence that is similar in position and decay properties to that of ScPO 4 crystals. Potentially this represents an STE in AlPO 4, and GaPO 4 crystals that is analogous to the STE of ScPO 4 and other orthophosphates. The decay kinetics of the UV luminescence of ScPO 4 were studied over a wide temperature range from 8 to 300 K, and they exhibited some unusual decay characteristics when subjected to pulses from an F 2 excimer laser (157 nm). These features could be ascribed to a triplet state of the STE that is split in a zero magnetic field. A fast decay of the STE was detected as well, and therefore, we conclude that, in addition to the slow luminescence corresponding to a transition from the triplet state, there are singlet-singlet transitions of the STE. Furthermore, time-resolved spectra of the slow and fast decay exhibit a small shift (~0.15 eV) indicating that the singlet triplet splitting is small and the corresponding wave function of the STE is widely distributed over the atoms of the ScPO 4 crystal where the STE is created.« less

Continuous Cooling from 10 K to 4 K Using a Toroidal ADR

NASA Technical Reports Server (NTRS)

DiPirro, Michael J.; Canavan, Edgar R.; Shirron, Peter J.; Tuttle, James G.

2003-01-01

Future large infrared space telescopes will require cooling to 4K to achieve background limited performance for submillimeter wavelengths. These observatories will require lifetimes of many years and will have relatively large cooling requirements making stored helium dewars impractical. We have designed and are building an adiabatic demagnetization refrigerator (ADR) for use in cooling relatively large loads (10- 100 mW) at 4K and rejecting that heat to a cryocooler operating at 1 OK. Cryocoolers below 1 OK have poor thermodynamic efficiency and ADRs can operate in this temperature range with an efficiency of 75% of Carnot or better. Overall, this can save as much as 2/3 of the input power required to operate a 4K cryocooler. The ADR magnet consists of 8 short coils wired in series and arranged in a toroid to provide self shielding of its magnetic field. This will save mass (about 30% of the mass or about 1.5 kg in our small version, higher percentages in higher cooling power, larger versions) that would have been used for passive or active shields in an ordinary solenoid. The toroid has a 100 mm outer diameter and will produce an approximately 3T average field. In the initial demonstration model the toroid coils will be wound with ordinary NbTi wire and operated at 4K. A second version will then use Nb3Sn wire to provide complete 10K operation. As a refrigerant for this temperature range we will use either GdLiF4 or GdF3 crystals, pending tests of these crystals' cooling capacity per field and thermal conductance. Preliminary indications are that these materials are superior to GGG. We will use gas gap heat switches to alternately connect the toroid to the cold load and the warm heat sink. A small continuous stage will maintain the cold end at 4K while the main toroid is recycled.

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

NASA Astrophysics Data System (ADS)

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

2010-01-01

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

Intricate Li-Sn Disorder in Rare-Earth Metal-Lithium Stannides. Crystal Chemistry of RE3Li4- xSn4+ x (RE = La-Nd, Sm; x < 0.3) and Eu7Li8- xSn10+ x ( x ≈ 2.0).

PubMed

Suen, Nian-Tzu; Guo, Sheng-Ping; Hoos, James; Bobev, Svilen

2018-05-07

Reported are the syntheses, crystal structures, and electronic structures of six rare-earth metal-lithium stannides with the general formulas RE 3 Li 4- x Sn 4+ x (RE = La-Nd, Sm) and Eu 7 Li 8- x Sn 10+ x . These new ternary compounds have been synthesized by high-temperature reactions of the corresponding elements. Their crystal structures have been established using single-crystal X-ray diffraction methods. The RE 3 Li 4- x Sn 4+ x phases crystallize in the orthorhombic body-centered space group Immm (No. 71) with the Zr 3 Cu 4 Si 4 structure type (Pearson code oI22), and the Eu 7 Li 8- x Sn 10+ x phase crystallizes in the orthorhombic base-centered space group Cmmm (No. 65) with the Ce 7 Li 8 Ge 10 structure type (Pearson code oC50). Both structures can be consdered as part of the [RESn 2 ] n [RELi 2 Sn] m homologous series, wherein the structures are intergrowths of imaginary RESn 2 (AlB 2 -like structure type) and RELi 2 Sn (MgAl 2 Cu-like structure type) fragments. Close examination the structures indicates complex occupational Li-Sn disorder, apparently governed by the drive of the structure to achieve an optimal number of valence electrons. This conclusion based on experimental results is supported by detailed electronic structure calculations, carried out using the tight-binding linear muffin-tin orbital method.

Crystallization and preliminary X-ray diffraction analysis of mouse galectin-4 N-terminal carbohydrate recognition domain in complex with lactose

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

Krejčiříková, Veronika; Fábry, Milan; Marková, Vladimíra

2008-07-01

Mouse galectin-4 carbohydrate binding domain was overexpressed in E. coli and crystallized in the presence of lactose. The crystals belong to tetragonal space group P42{sub 1}2 and diffraction data were collected to 2.1 Å resolution. Galectin-4 is thought to play a role in the process of tumour conversion of cells of the alimentary tract and the breast tissue; however, its exact function remains unknown. With the aim of elucidating the structural basis of mouse galectin-4 (mGal-4) binding specificity, we have undertaken X-ray analysis of the N-terminal domain, CRD1, of mGal-4 in complex with lactose (the basic building block of knownmore » galectin-4 carbohydrate ligands). Crystals of CRD1 in complex with lactose were obtained using vapour-diffusion techniques. The crystals belong to tetragonal space group P42{sub 1}2 with unit-cell parameters a = 91.1, b = 91.16, c = 57.10 Å and preliminary X-ray diffraction data were collected to 3.2 Å resolution. An optimized crystallization procedure and cryocooling protocol allowed us to extend resolution to 2.1 Å. Structure refinement is currently under way; the initial electron-density maps clearly show non-protein electron density in the vicinity of the carbohydrate binding site, indicating the presence of one lactose molecule. The structure will help to improve understanding of the binding specificity and function of the potential colon cancer marker galectin-4.« less

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.

Structure and crystallization of SiO2 and B2O3 doped lithium disilicate glasses from theory and experiment.

PubMed

Erlebach, Andreas; Thieme, Katrin; Sierka, Marek; Rüssel, Christian

2017-09-27

Solid solutions of SiO 2 and B 2 O 3 in Li 2 O·2SiO 2 are synthesized and characterized for the first time. Their structure and crystallization mechanisms are investigated employing a combination of simulations at the density functional theory level and experiments on the crystallization of SiO 2 and B 2 O 3 doped lithium disilicate glasses. The remarkable agreement of calculated and experimentally determined cell parameters reveals the preferential, kinetically controlled incorporation of [SiO 4 ] and [BO 4 ] at the Li + lattice sites of the Li 2 O·2SiO 2 crystal structure. While the addition of SiO 2 increases the glass viscosity resulting in lower crystal growth velocities, glasses containing B 2 O 3 show a reduction of both viscosities and crystal growth velocities. These observations could be rationalized by a change of the chemical composition of the glass matrix surrounding the precipitated crystal phase during the course of crystallization, which leads to a deceleration of the attachment of building units required for further crystal growth at the liquid-crystal interface.

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

Yeh, G.P.; /Fermilab

Studies of requirements and specifications of crystals are necessary to develop a new generation of crystals for dual readout crystal hadron or total absorption calorimeter. This is a short and basic study of the characteristics and hadron energy measurement of PbWO4 and BGO crystals for scintillation and Cerenkov Dual Readout hadron calorimeter.

Reinjury risk of nano-calcium oxalate monohydrate and calcium oxalate dihydrate crystals on injured renal epithelial cells: aggravation of crystal adhesion and aggregation

PubMed Central

Gan, Qiong-Zhi; Sun, Xin-Yuan; Bhadja, Poonam; Yao, Xiu-Qiong; Ouyang, Jian-Ming

2016-01-01

Background Renal epithelial cell injury facilitates crystal adhesion to cell surface and serves as a key step in renal stone formation. However, the effects of cell injury on the adhesion of nano-calcium oxalate crystals and the nano-crystal-induced reinjury risk of injured cells remain unclear. Methods African green monkey renal epithelial (Vero) cells were injured with H2O2 to establish a cell injury model. Cell viability, superoxide dismutase (SOD) activity, malonaldehyde (MDA) content, propidium iodide staining, hematoxylin–eosin staining, reactive oxygen species production, and mitochondrial membrane potential (Δψm) were determined to examine cell injury during adhesion. Changes in the surface structure of H2O2-injured cells were assessed through atomic force microscopy. The altered expression of hyaluronan during adhesion was examined through laser scanning confocal microscopy. The adhesion of nano-calcium oxalate monohydrate (COM) and calcium oxalate dihydrate (COD) crystals to Vero cells was observed through scanning electron microscopy. Nano-COM and COD binding was quantitatively determined through inductively coupled plasma emission spectrometry. Results The expression of hyaluronan on the cell surface was increased during wound healing because of Vero cell injury. The structure and function of the cell membrane were also altered by cell injury; thus, nano-crystal adhesion occurred. The ability of nano-COM to adhere to the injured Vero cells was higher than that of nano-COD crystals. The cell viability, SOD activity, and Δψm decreased when nano-crystals attached to the cell surface. By contrast, the MDA content, reactive oxygen species production, and cell death rate increased. Conclusion Cell injury contributes to crystal adhesion to Vero cell surface. The attached nano-COM and COD crystals can aggravate Vero cell injury. As a consequence, crystal adhesion and aggregation are enhanced. These findings provide further insights into kidney stone formation. PMID:27382277

Fluorescent Approaches to High Throughput Crystallography

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Forsythe, Elizabeth; Achari, Amiruddha

2005-01-01

X-ray crystallography remains the primary method for determining the structure of macromolecules. The first requirement is to have crystals, and obtaining them is often the rate-limiting step. The numbers of crystallization trials that are set up for any one protein for structural genomics, and the rate at which they are being set up, now overwhelm the ability for strictly human analysis of the results. Automated analysis methods are now being implemented with varying degrees of success, but these typically cannot reliably extract intermediate results. By covalently modifying a subpopulation, less than or = 1 %, of a macromolecule solution with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of purification. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination the crystals show up as bright objects against a dark background. As crystalline packing is more dense than amorphous precipitate, the fluorescence intensity can be used as a guide in distinguishing different types of precipitated phases, even in the absence of obvious crystalline features, widening the available potential lead conditions in the absence of clear "hits." Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Also, brightly fluorescent crystals are readily found against less fluorescent precipitated phases, which under white light illumination may serve to obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries and by having the protein or protein structures all that show up. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons. Preliminary experiments show that the presence of the fluorescent probe does not affect the nucleation process or the quality of the X-ray data obtained.

Fluorescent Applications to Crystallization

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Forsythe, Elizabeth; Achari, Aniruddha

2006-01-01

By covalently modifying a subpopulation, less than or equal to 1%, of a macromolecule with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of purification, and tests with model proteins have shown that labeling u to 5 percent of the protein molecules does not affect the X-ray data quality obtained . The presence of the trace fluorescent label gives a number of advantages. Since the label is covalently attached to the protein molecules, it "tracks" the protein s response to the crystallization conditions. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination crystals show up as bright objects against a darker background. Non-protein structures, such as salt crystals, do not show up under fluorescent illumination. Crystals have the highest protein concentration and are readily observed against less bright precipitated phases, which under white light illumination may obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries as the protein or protein structures is all that shows up. Fluorescence intensity is a faster search parameter, whether visually or by automated methods, than looking for crystalline features. Preliminary tests, using model proteins, indicates that we can use high fluorescence intensity regions, in the absence of clear crystalline features or "hits", as a means for determining potential lead conditions. A working hypothesis is that more rapid amorphous precipitation kinetics may overwhelm and trap more slowly formed ordered assemblies, which subsequently show up as regions of brighter fluorescence intensity. Experiments are now being carried out to test this approach using a wider range, of proteins. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons.