Scheelite distribution a long of amphibolitic belt from greenstone belt Barbacena, Minas Gerais, Brazil

International Nuclear Information System (INIS)

Pereira, R.M.; Alexandre, C.A.

1990-01-01

In the middle southern portion of the Minas Gerais state a 60 Km long and 12 Km wide tungsten belt was discovered, and related to the amphibolitic rocks of the Barbacena Greenstone. Tungsten, present as scheelite, is associated with amphibolites, amphibole schists and amphibole gneisses, with chemical characteristics indicating an igneous origin. Chemical analyses on pan concentrates by I.C.P. showed high values on lead, tin, yttrium, lanthanum, cerium and zirconium, and average values for zinc and copper. The scheelite mineralization is probably strata bound and has a possible submarine exhalative origin. (author)

Study on the Activation of Scheelite and Wolframite by Lead Nitrate

Directory of Open Access Journals (Sweden)

Gang Zhao

2015-04-01

Full Text Available The activation of scheelite and wolframite by lead nitrate with benzohydroxamic acid (BHA as collector was investigated by means of micro flotation test, zeta potential measurement, X-ray photoelectron spectroscopy (XPS analyses and density functional theory (DFT calculation. The flotation results confirmed that the addition of lead nitrate can markedly enhance the recovery of scheelite and wolframite. In the zeta potential curves obvious positive shifts were observed with the presence of lead nitrate. Lead was detected on mineral surface in microscopic analysis and the survey XP spectra. Both the electrokinetic study and XPS analyses indicated that lead ion can be adsorbed onto mineral surface. In DFT calculation, the coordination model of BHA with metal hydroxyl ions (Ca(OH+, Mn(OH+, Fe(OH+ and Pb(OH+ was simulated and their binding energy were also calculated. The calculated results revealed that the binding ability of BHA and Pb(OH+ is the strongest, indicating that BHA can preferentially coordinate with Pb ion compared with Ca, Mn and Fe ions.

A study of electron excitations in CaWO sub 4 and PbWO sub 4 single crystals

CERN Document Server

Muerk, V; Mihoková, E; Nitsch, K

1997-01-01

The excitation spectra of photo- and thermo-luminescence were compared in the VUV-UV spectral region in CaWO sub 4 and PbWO sub 4 scheelite tungstates. Temperature dependences of emission intensities and decay times were measured for PbWO sub 4 in the 80-300 K range and approximated by a simple phenomenological model. The energy level structure of the emission centre excited state and related kinetic processes are discussed for both tungstates. (author)

Pressure-induced phase transformation in zircon-type orthovanadate SmVO4 from experiment and theory

International Nuclear Information System (INIS)

Popescu, C; Garg, Alka B; Errandonea, D; Sans, J A; Rodriguez-Hernández, P; Radescu, S; Muñoz, A; Achary, S N; Tyagi, A K

2016-01-01

The compression behavior of zircon-type samarium orthovanadate, SmVO 4 , has been investigated using synchrotron-based powder x-ray diffraction and ab initio calculations of up to 21 GPa. The results indicate the instability of ambient zircon phase at around 6 GPa, which transforms to a high-density scheelite-type phase. The high-pressure phase remains stable up to 21 GPa, the highest pressure reached in the present investigations. On pressure release, the scheelite phase is recovered. The crystal structure of the high-pressure phase and the equations of state for the zircon- and scheelite-type phases have been determined. Various compressibilities, such as the bulk, axial and bond compressibilities, estimated from the experimental data are found to be in good agreement with the results obtained from theoretical calculations. The calculated elastic constants show that the zircon structure becomes mechanically unstable beyond the transition pressure. Overall there is good agreement between the experimental and theoretical findings. (paper)

Acid leaching of scheelite concentrates; Lixiviacion acida de concentrado de scheelita

Energy Technology Data Exchange (ETDEWEB)

Navarro, P.; Vargas, C.; Alguacil, F. J.

2005-07-01

The acid leaching in hydrochloric media of a tungsten concentrate (scheelite, CaWO{sub 4}) was studied. Of the above-mentioned, an insoluble solid (H{sub 2}WO{sub 4}) was obtained which were treated with an alkaline solution of sodium hydroxide, achieving the complete solubilization of the tungsten as wolframate ion (WO''2{sub 4}). The transformed fraction of tungsten increases with the temperature, as well as with a finer grain. A maximum dissolution of 88.5% (400 g/l HCL, 363 K and 20 {mu}m of particle size) was achieved for a 3 h process, of the dissolution process was interpreted by the recessive core model with formation of a layer of solid product for the whole range of variation of the parameters in study. the activation energy value was found to be 28.0kJ/mol. (Author) 6 refs.

High pressure Raman scattering study on the phase stability of LuVO4

International Nuclear Information System (INIS)

Rao, Rekha; Garg, Alka B.; Sakuntala, T.; Achary, S.N.; Tyagi, A.K.

2009-01-01

High pressure Raman spectroscopic investigations have been carried out on rare earth orthovanadate LuVO 4 upto 26 GPa. Changes in the Raman spectrum around 8 GPa across the reported zircon to scheelite transition are investigated in detail and compared with those observed in other vanadates. Co-existence of the zircon and scheelite phases is observed over a pressure range of about 8-13 GPa. The zircon to scheelite transition is irreversible upon pressure release. Subtle changes are observed in the Raman spectrum above 16 GPa which could be related to scheelite ↔ fergusonite transition. Pressure dependencies of the Raman active modes in the zircon and the scheelite phases are reported. - Graphical abstract: Study of scheelite-fergusonite transition in RVO 4 by Raman spectroscopy is rare. Here we report Raman spectroscopic investigations of LuVO 4 at high pressure to obtain insight into nature of post-scheelite phases.

Zeta-potential and flotability of the scheelite mineral in different type of waters, Part 1: Zeta-potential

Directory of Open Access Journals (Sweden)

Milanović Dragan B.

2009-01-01

Full Text Available The aim of this work is the investigation of zeta-potential of the mineral scheelite from mine 'Rudnik', located in central Serbia. Electrophoresis measurements using zeta-meter were carried out on four different types of water, namely: tap water, distilled water, rain water and spring water. All types of water had different hardness and conductivity as well as natural pH values. It was found that the zeta-potential of mineral scheelite depends on the hardness and electro-conductivity of the chosen type of water as well as on Ca2+ content. The results obtained reveal the importance of proper choice of water as well as the type of reagents for flotation processes.

Zeta-potential and flotability of the scheelite mineral in different type of waters, Part 2: Flotability

Directory of Open Access Journals (Sweden)

Milanović Dragan B.

2009-01-01

Full Text Available The aim of this work was to study floatability of the mineral sheelite from mine 'Rudnik', central Serbia. Flotation tests of the mineral in a Hallimond tube cell were carried out in four different types of water, namely: tap water, distilled water, rain water and spring water. All types of water had different hardness and conductivity as well as natural pH values. It was found that the flotability of mineral scheelite depends on the hardness and electro-conductivity of the chosen type of water as well as on Ca2+ content. Also, it was found the floatability of mineral depends on the scheelite particle size fraction used in microflotation experiments. Presented results may be useful for proper selection of type of water, as well of the type of reagents used in flotation processes.

On the photo-luminescence properties of sol–gel derived undoped and Dy3+ ion doped nanocrystalline Scheelite type AMoO4 (A = Ca, Sr and Ba)

International Nuclear Information System (INIS)

Jena, Paramananda; Gupta, Santosh K.; Natarajan, V.; Padmaraj, O.; Satyanarayana, N.; Venkateswarlu, M.

2015-01-01

Nanocrystalline Scheelite type Dy doped AMoO 4 [where A = Ba, Sr and Ca] samples were prepared by acrylamide assisted sol–gel process and characterized by XRD, FT-Raman, FTIR, SEM and photoluminescence (PL). PL of undoped sample shows blue/green emission in CaMoO 4 and SrMoO 4 but multicolour visible emission leading to near white light in BaMoO 4 nanoparticles; the origin of which is explained. It was observed that on doping 0.5 mol% of Dy 3+ in molybdate samples complete energy transfer takes place in case of SrMoO 4 and BaMoO 4 , but host contributed substantially in Dy doped BaMoO 4 sample, resulting in biexponential decay. It was also observed that symmetry around Dy 3+ decreases as the size of alkaline earth ion increases. Due to combined blue, yellow and red colour emission in dysprosium doped sample; all samples showed near white light emission under UV and near UV excitation

SrWO4 at high pressures

International Nuclear Information System (INIS)

Grzechnik, A.; Crichton, W.A.; Hanfland, M.

2005-01-01

Room-temperature high-pressure behaviour of SrWO 4 scheelite (I4 1 /a, Z=4) has been studied to 20.7 GPa in a diamond anvil cell using synchrotron angle-dispersive X-ray powder diffraction. Above 10 GPa, it transforms to the fergusonite structure (I2/a, Z=4). Both scheelite and fergusonite types are ordered superstructures of fluorite (Fm anti 3m, Z=4). There is no significant volume collapse at the scheelite-fergusonite phase transition. However, the compression data including both phases of strontium tungstate cannot be fitted by a common Birch-Murnaghan equation of state. An onset of decomposition into component oxides occurs at about 15 GPa. The pressure-induced transformations are irreversible. (copyright 2005 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

SrWO{sub 4} at high pressures

Energy Technology Data Exchange (ETDEWEB)

Grzechnik, A. [Departamento de Fisica de la Materia Condensada, Universidad del Pais Vasco, Apdo. 644, Bilbao 48080 (Spain); European Synchrotron Radiation Facility, B.P. 220, 38043 Grenoble cedex (France); Crichton, W.A.; Hanfland, M. [European Synchrotron Radiation Facility, B.P. 220, 38043 Grenoble cedex (France)

2005-11-01

Room-temperature high-pressure behaviour of SrWO{sub 4} scheelite (I4{sub 1}/a, Z=4) has been studied to 20.7 GPa in a diamond anvil cell using synchrotron angle-dispersive X-ray powder diffraction. Above 10 GPa, it transforms to the fergusonite structure (I2/a, Z=4). Both scheelite and fergusonite types are ordered superstructures of fluorite (Fm anti 3m, Z=4). There is no significant volume collapse at the scheelite-fergusonite phase transition. However, the compression data including both phases of strontium tungstate cannot be fitted by a common Birch-Murnaghan equation of state. An onset of decomposition into component oxides occurs at about 15 GPa. The pressure-induced transformations are irreversible. (copyright 2005 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

The determination, by x-ray-fluorescence spectrometry, of tin and tungsten in scheelite and cassiterite ores and concentrates

International Nuclear Information System (INIS)

Tolmay, R.T.; Jacobs, J.J.

1980-01-01

A method of analysis is presented that is applicable to sample mixtures of cassiterite and scheelite in concentrations of 0,2 to 70 per cent. Matrix variations are compensated for by dilution and fine grinding with coarse river sand, potassium chloride being used as a binder. Residual matrix effects are corrected for by the use of zinc and antimony as internal standards for tungsten and tin respectively. Calibration graphs are obtained by the use of chemically analysed scheelite and cassiterite standards. For tin, the relative standard deviation at a concentration of 60 per cent is 0,0063, and, at 10 per cent, 0,028; for tungsten, it is 0,013 at a concentration of 40 per cent. The lower levels of detection for tungsten and tin are 0,26 and 0,23 per cent respectively, and the time required for the analysis of 10 samples and 5 calibration standards by this method is 5 hours. A detailed laboratory method is given in the appendix [af

Phase equilibria in the CdMoO4-Gd2(MoO4)3 system

International Nuclear Information System (INIS)

Tunik, T.A.; Fedorov, N.F.; Razumovskij, S.N.

1980-01-01

The constitutional diagram of the CdMoO 4 -Cd 2 (MoO 4 ) 3 system has been plotted using statistical and dynamic methods as well as a complex of instrumental analysis procedures. Three major phases have been found to occur in the systems, viz.: CdMoO 4 based solid solutions that crystallize in the range from 0 to 25 mol.percent of Cd 2 (MoO 4 ) 3 and pass in transit the two-phase narrow region becoming then solid solutions having a distorted scheelite structure and existing in concentrations from 40 to 65 mol.% of Cd 2 (MoO 4 ) 3 . The entire range, in which the Cd 2 (MoO 4 ) 3 solid solutions can exist, amounts to less than 5 mol.%. Certain crystallochemical constants of the phases that occur in the system have been determined [ru

High-pressure polymorphs of TbVO4: A Raman and ab initio study

International Nuclear Information System (INIS)

Errandonea, D.; Manjón, F.J.; Muñoz, A.; Rodríguez-Hernández, P.; Panchal, V.; Achary, S.N.; Tyagi, A.K.

2013-01-01

Highlights: •Three phase transitions are induced in zircon-type TbVO4 at 6.7, 26.7, and 34.4 GPa. •The proposed structural sequence is zircon-scheelite-fergusonite-orthorhombic Cmca. •Scheelite phase is metaestable after decompression. •The equation of states for all phases is reported. •Compressibility is enhanced in the Cmca phase due to f-electron delocalization. -- Abstract: Raman measurements on TbVO 4 show the occurrence of three pressure-induced phase transitions. The first one, an irreversible transition from the zircon to the scheelite structure, occurs beyond 6.7 GPa. In addition, two reversible transformations take place at 26.7 and 34.4 GPa. The last transition was never reported before. The experimental findings are supported by structural and lattice-dynamics calculations that helped us to identify the post-scheelite phase as a monoclinic fergusonite structure. According to the calculations, the third transition involves a symmetry increase. An orthorhombic structure is proposed for the phase found above 34.4 GPa. The results have been compared with previous studies in TbVO 4 and discussed in comparison with related compounds. The calculated equations of state are reported for the different polymorphs of TbVO 4 . A compressibility increase is caused by the third transition. It is associated to a bond-strength decrease, which is related to a coordination increase and a delocalization of Tb f-electrons

Equation of state and electronic properties of EuVO4: A high-pressure experimental and computational study

International Nuclear Information System (INIS)

Paszkowicz, Wojciech; López-Solano, Javier; Piszora, Paweł; Bojanowski, Bohdan; Mujica, Andrés; Muñoz, Alfonso; Cerenius, Yngve; Carlson, Stefan; Dąbkowska, Hanna

2015-01-01

Structural, elastic and electronic properties of zircon-type and scheelite-type EuVO 4 are investigated experimentally, by in-situ X-ray diffraction using synchrotron radiation, and theoretically within the framework of the density functional theory (DFT) and using the PBE prescription of the exchange-correlation energy. This study was motivated by the fact that the previous knowledge of the equation of state (EOS) was inconclusive due to a large scatter of the experimental and theoretical data, and by the lack of information on the dependence of the electronic structure with pressure. Under the applied experimental conditions, the zircon-type structure transforms to a scheelite-type one at 7.4(2) GPa, whereas the calculations yield a lower zircon–scheelite-coexistence pressure of 4.8 GPa. The experimental part of the study shows that the bulk modulus of the zircon-type phase is 119(3) GPa, perfectly supported by the DFT-calculated value, 119.1 GPa. The bulk modulus for the scheelite-type polymorph is higher, with an experimental value of 135(7) GPa and a theoretical one of 137.4 GPa. Compared to those reported in previous experimental and DFT or semiempirical works, the present values for the zircon-type phase are comparable or slightly lower, whereas those for the scheelite-type phase are markedly lower. Discrepancies between the present results and earlier reported ones are attributed to differences in details of the experimental method such as the pressure transmitting medium and the pressure calibration method. The calculated band structure confirms that zircon-type EuVO 4 is a direct-gap semiconductor, with a bandgap energy at zero pressure of 2.88 eV. Under compression, the bandgap of the zircon phase increases with a coefficient of 10.3 meV/GPa up to the transition pressure, at which point the present calculations show a small drop of the bandgap energy. Above the transition pressure, the bandgap energy of the scheelite phase becomes almost constant, with

High-pressure polymorphs of TbVO{sub 4}: A Raman and ab initio study

Energy Technology Data Exchange (ETDEWEB)

Errandonea, D., E-mail: daniel.errandonea@uv.es [Departamento de Física Aplicada-ICMUV, Universidad de Valencia, MALTA Consolider Team, Edificio de Investigación, C/Dr. Moliner 50, Burjassot, 46100 Valencia (Spain); Manjón, F.J. [Instituto de Diseño para la Fabricación y Producción Automatizada, MALTA Consolider Team, Universidad Politécnica de Valencia, Camino de Vera s/n, 46022 Valencia (Spain); Muñoz, A.; Rodríguez-Hernández, P. [Departamento de Física Fundamental II, Instituto de Materiales y Nanotecnología, MALTA Consolider Team, Universidad de La Laguna, La Laguna 38205, Tenerife (Spain); Panchal, V. [Departamento de Física Aplicada-ICMUV, Universidad de Valencia, MALTA Consolider Team, Edificio de Investigación, C/Dr. Moliner 50, Burjassot, 46100 Valencia (Spain); Royal College of Arts, Science and Commerce, Mira Road, Mumbai 401 107 (India); Achary, S.N.; Tyagi, A.K. [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085 (India)

2013-11-15

Highlights: •Three phase transitions are induced in zircon-type TbVO4 at 6.7, 26.7, and 34.4 GPa. •The proposed structural sequence is zircon-scheelite-fergusonite-orthorhombic Cmca. •Scheelite phase is metaestable after decompression. •The equation of states for all phases is reported. •Compressibility is enhanced in the Cmca phase due to f-electron delocalization. -- Abstract: Raman measurements on TbVO{sub 4} show the occurrence of three pressure-induced phase transitions. The first one, an irreversible transition from the zircon to the scheelite structure, occurs beyond 6.7 GPa. In addition, two reversible transformations take place at 26.7 and 34.4 GPa. The last transition was never reported before. The experimental findings are supported by structural and lattice-dynamics calculations that helped us to identify the post-scheelite phase as a monoclinic fergusonite structure. According to the calculations, the third transition involves a symmetry increase. An orthorhombic structure is proposed for the phase found above 34.4 GPa. The results have been compared with previous studies in TbVO{sub 4} and discussed in comparison with related compounds. The calculated equations of state are reported for the different polymorphs of TbVO{sub 4}. A compressibility increase is caused by the third transition. It is associated to a bond-strength decrease, which is related to a coordination increase and a delocalization of Tb f-electrons.

Equation of state and electronic properties of EuVO{sub 4}: A high-pressure experimental and computational study

Energy Technology Data Exchange (ETDEWEB)

Paszkowicz, Wojciech, E-mail: paszk@ifpan.edu.pl [Institute of Physics, Polish Academy of Sciences, al. Lotników 32/46, 02-668 Warsaw (Poland); López-Solano, Javier [Departamento de Física, MALTA Consolider Team, and Instituto de Materiales y Nanotecnología, Universidad de La Laguna, Tenerife 38205 (Spain); Izaña Atmospheric Research Center, Agencia Estatal de Meteorología (AEMET), Tenerife 38071 (Spain); Piszora, Paweł [Department of Materials Chemistry, Faculty of Chemistry, Adam Mickiewicz University, Umultowska 89b, 61-614 Poznań (Poland); Bojanowski, Bohdan [Institute of Physics, Szczecin University of Technology, Aleja Piastów 48, 70-310 Szczecin (Poland); Mujica, Andrés; Muñoz, Alfonso [Departamento de Física, MALTA Consolider Team, and Instituto de Materiales y Nanotecnología, Universidad de La Laguna, Tenerife 38205 (Spain); Cerenius, Yngve; Carlson, Stefan [MAX IV Laboratory, Lund University, P.O. Box 118, SE-221 00 Lund (Sweden); Dąbkowska, Hanna [Brockhouse Institute for Materials Research, McMaster University, Hamilton, Ontario L8S 4M1 (Canada)

2015-11-05

Structural, elastic and electronic properties of zircon-type and scheelite-type EuVO{sub 4} are investigated experimentally, by in-situ X-ray diffraction using synchrotron radiation, and theoretically within the framework of the density functional theory (DFT) and using the PBE prescription of the exchange-correlation energy. This study was motivated by the fact that the previous knowledge of the equation of state (EOS) was inconclusive due to a large scatter of the experimental and theoretical data, and by the lack of information on the dependence of the electronic structure with pressure. Under the applied experimental conditions, the zircon-type structure transforms to a scheelite-type one at 7.4(2) GPa, whereas the calculations yield a lower zircon–scheelite-coexistence pressure of 4.8 GPa. The experimental part of the study shows that the bulk modulus of the zircon-type phase is 119(3) GPa, perfectly supported by the DFT-calculated value, 119.1 GPa. The bulk modulus for the scheelite-type polymorph is higher, with an experimental value of 135(7) GPa and a theoretical one of 137.4 GPa. Compared to those reported in previous experimental and DFT or semiempirical works, the present values for the zircon-type phase are comparable or slightly lower, whereas those for the scheelite-type phase are markedly lower. Discrepancies between the present results and earlier reported ones are attributed to differences in details of the experimental method such as the pressure transmitting medium and the pressure calibration method. The calculated band structure confirms that zircon-type EuVO{sub 4} is a direct-gap semiconductor, with a bandgap energy at zero pressure of 2.88 eV. Under compression, the bandgap of the zircon phase increases with a coefficient of 10.3 meV/GPa up to the transition pressure, at which point the present calculations show a small drop of the bandgap energy. Above the transition pressure, the bandgap energy of the scheelite phase becomes almost

First-order character of the displacive structural transition in BaWO4

International Nuclear Information System (INIS)

Tan Da-Yong; Xiao Wan-Sheng; Zhou Wei; Chen Ming; Xiong Xiao-Lin; Song Mao-Shuang

2012-01-01

Nearly all displacive transitions have been considered to be continuous or second order, and the rigid unit mode (RUM) provides a natural candidate for the soft mode. However, in-situ X-ray diffraction and Raman measurements show clearly the first-order evidences for the scheelite-to-fergusonite displacive transition in BaWO 4 : a 1.6% volume collapse, coexistence of phases, and hysteresis on release of pressure. Such first-order signatures are found to be the same as the soft modes in BaWO 4 , which indicates the scheelite-to-fergusonite displacive phase transition hides a deeper physical mechanism. By the refinement of atomic displacement parameters, we further show that the first-order character of this phase transition stems from a coupling of large compression of soft BaO 8 polyhedrons to the small displacive distortion of rigid WO 4 tetrahedrons. Such a coupling will lead to a deeper physical insight in the phase transition of the common scheelite-structured compounds. (condensed matter: structural, mechanical, and thermal properties)

Petrogenesis of postcollisional magmatism at Scheelite Dome, Yukon, Canada: Evidence for a lithospheric mantle source for magmas associated with intrusion-related gold systems

Science.gov (United States)

Mair, John L.; Farmer, G. Lang; Groves, David I.; Hart, Craig J.R.; Goldfarb, Richard J.

2011-01-01

The type examples for the class of deposits termed intrusion-related gold systems occur in the Tombstone-Tungsten belt of Alaska and Yukon, on the eastern side of the Tintina gold province. In this part of the northern Cordillera, extensive mid-Cretaceous postcollisional plutonism took place following the accretion of exotic terranes to the continental margin. The most cratonward of the resulting plutonic belts comprises small isolated intrusive centers, with compositionally diverse, dominantly potassic rocks, as exemplified at Scheelite Dome, located in central Yukon. Similar to other spatially and temporally related intrusive centers, the Scheelite Dome intrusions are genetically associated with intrusion-related gold deposits. Intrusions have exceptional variability, ranging from volumetrically dominant clinopyroxene-bearing monzogranites, to calc-alkaline minettes and spessartites, with an intervening range of intermediate to felsic stocks and dikes, including leucominettes, quartz monzonites, quartz monzodiorites, and granodiorites. All rock types are potassic, are strongly enriched in LILEs and LREEs, and feature high LILE/HFSE ratios. Clinopyroxene is common to all rock types and ranges from salite in felsic rocks to high Mg augite and Cr-rich diopside in lamprophyres. Less common, calcic amphibole ranges from actinolitic hornblende to pargasite. The rocks have strongly radiogenic Sr (initial 87Sr/86Sr from 0.711-0.714) and Pb isotope ratios (206Pb/204Pb from 19.2-19.7), and negative initial εNd values (-8.06 to -11.26). Whole-rock major and trace element, radiogenic isotope, and mineralogical data suggest that the felsic to intermediate rocks were derived from mafic potassic magmas sourced from the lithospheric mantle via fractional crystallization and minor assimilation of metasedimentary crust. Mainly unmodified minettes and spessartites represent the most primitive and final phases emplaced. Metasomatic enrichments in the underlying lithospheric mantle

Study of reverse flotation of calcite from scheelite in acidic media

Science.gov (United States)

Deng, Rongdong; Huang, Yuqing; Hu, Yuan; Ku, Jiangang; Zuo, Weiran; Yin, Wanzhong

2018-05-01

A new coated-reactive reverse flotation method based on the generation of CO2 bubbles at a calcite surface in acidic solution was used to separate calcite from scheelite. The dissolution kinetics of coated and uncoated calcite were studied in sulfuric acid. The CO2 bubbles generated on the uncoated calcite particle surface are enough to float the particle. However, most of these bubbles left the surface quickly, preventing calcite from floating. Here, a mixture of polyvinyl alcohol polymer and sodium dodecyl sulfonate was used to coat the mineral particles and form a stable membrane, resulting in the formation of a stable foam layer on the calcite surface. After the calcite is coated, the generated bubbles could be successfully captured on the calcite surface, and calcite particles could float to the air-water interface and remain there for more than one hour. Flotation tests indicated that a high-quality tungsten concentrate with a grade of more than 75% and a recovery of more than 99% could be achieved when the particle size was between 0.3 and 1.5 mm. The present results provide theoretical support for the development of a highly efficient flotation separation for carbonate minerals.

Crystal growth and properties of novel organic nonlinear optical crystals of 4-Nitrophenol urea

Energy Technology Data Exchange (ETDEWEB)

Mohan, M. Krishna, E-mail: krishnamohan.m@ktr.srmuniv.ac.in; Ponnusamy, S.; Muthamizhchelvan, C.

2017-07-01

Single crystals of 4-Nitrophenol urea have been grown from water using slow evaporation technique at constant temperature, with the vision to improve the properties of the crystals. The unit cell parameters of the grown crystals were determined by single crystal and powder X-Ray diffraction. FTIR studies reveals the presence of different vibrational bands. The Optical studies confirmed that the crystal is transparent up to 360 nm .TGA and DSC studies were carried out to understand the thermal behavior of crystals. The SHG studies show the suitability of the crystals for NLO applications. The etching studies were carried out to study the behavior of the crystals under different conditions.These studies reveal that the crystals of 4-Nitrophenol urea are suitable for device applications. - Highlights: • 4-Nitrophenol urea crystals of dimensions 14 mm × 1 mm were grown. • UV–Visible studies indicate the crystal is transparent in the region of 370–800 nm. • Thermal studies show the crystal starts decomposing at 170 °C. • SHG studies indicate that the crystals have NLO efficiency 3.5 times that of KDP.

Crystal structures of 4-methoxy-N-(4-methylphenylbenzenesulfonamide and N-(4-fluorophenyl-4-methoxybenzenesulfonamide

Directory of Open Access Journals (Sweden)

Vinola Z. Rodrigues

2015-11-01

Full Text Available Crystal structures of two N-(arylarylsulfonamides, namely, 4-methoxy-N-(4-methylphenylbenzenesulfonamide, C14H15NO3S, (I, and N-(4-fluorophenyl-4-methoxybenzenesulfonamide, C13H12FNO3S, (II, were determined and analyzed. In (I, the benzenesulfonamide 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 intermolecular C—H...πaryl interactions 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 intermolecular interactions consolidate the crystal packing of (II into a three-dimensional supramolecular architecture.

Optical lines in europium-terbium double activated calcium tungstate phosphor

Energy Technology Data Exchange (ETDEWEB)

Nazarov, M.V. [Department of Material Science and Engineering, Korea Advanced Institute of Science and Technology, 373-1 Guseong-dong, Yuseong-gu, Daejeon 305-701 (Korea, Republic of); Tsukerblat, B.S. [Department of Chemistry, Ben-Gurion University of the Negev, 84105 Beer-Sheva (Israel)]. E-mail: tsuker@bgumail.bgu.ac.il; Popovici, E.-J. [' Raluca Ripan' Institute for Research in Chemistry, Cluj-Napoca (Romania); Jeon, D.Y. [Department of Material Science and Engineering, Korea Advanced Institute of Science and Technology, 373-1 Guseong-dong, Yuseong-gu, Daejeon 305-701 (Korea, Republic of)

2004-09-20

The Letter is devoted to the problem of the optical anisotropy of the rare-earth ions occupying low-symmetry positions in crystals. The crystal field multiplets arising from LSJ terms of Eu{sup 3+} and Tb{sup 3+} ions in the crystal field of calcium tungstate scheelite (CaWO{sub 4}) are analyzed with regard to the experimental data on the low temperature photoluminescence and cathodoluminescence spectra. The selection rules as well as an angular (polarization) dependence of the two-photon absorption are discussed.

Progress in PbWO4 scintillating crystal

International Nuclear Information System (INIS)

Fyodorov, A.; Korzhik, M.; Missevitch, O.; Pavlenko, V.; Kachanov, V.; Singovsky, A.; Annenkov, A.N.; Ligun, V.A.; Peigneux, J.P.; Vialle, J.P.

1994-12-01

Lead tungstate PbWO 4 (PWO) has recently been shown to be a promising scintillating material for precise electromagnetic calorimetry. Modifications of PWO technology were made to improve the uniformity of the crystal properties. A model of the scintillation mechanism for PWO was developed and served to guide the improvement. The complex spectroscopic analysis of the crystal after improvement is presented, as well as the new crystal properties achieved. (K.A.). 14 refs., 14 figs., 4 tabs

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

Science.gov (United States)

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.

Spin-phonon and lattice contributions to the ground-state splitting of Gd3+ and Eu2+ in scheelite crystals

Science.gov (United States)

Gorlov, A. D.

2015-07-01

The EPR spectra of Gd3+ in CaWO4 single crystals have been studied at temperatures T = 1.8, 4.2, and 114-300 K, and the temperature dependence of the parameters b {/n m } ( T) of the spin Hamiltonian has been found. The behavior of b {2/0}( T) has been analyzed. The spin-phonon and static lattice contributions b {2/0}( F) and b {2/0}( L) to b {2/0}( T) have been revealed. For this purpose, the variation of b {2/0}( L) has been calculated taking into account the thermal shifts of oxygen ions in CaWO4. Similar analysis has been carried out for CaWO4: Eu2+ based on the EPR data of other authors (Bronstein, Voterra and Harvey, Kiefte). It has been shown that at b {2/0}( F) > 0, the variation of b {2/0}( F) as a function of T for these impurity centers is described well by the Pfister model and a sign change of b {2/0}( T) for Eu2+ is determined by thermal expansion of the lattice.

Monoclinic mixed crystals of halogenomethanes CBr4-nCln (n = 0, ..., 4)

International Nuclear Information System (INIS)

Negrier, Philippe; Tamarit, Josep Ll.; Barrio, Maria; Pardo, Luis C.; Mondieig, Denise

2007-01-01

On the basis of the isostructural relationship between the low-temperature monoclinic (C2/c, Z = 32) phases of the halogenomethane CBr 4-n Cl n (n = 0, ..., 4), a set of mixed crystals has been analysed by means of high-resolution X-ray powder diffraction. It is shown that the monoclinic structure of pure and mixed crystals does not depend of the particularities of the dipolar (or dipole induced) interactions of the pure compound, neither on the composition of the mixed crystal, but on the relative content of the halogen atoms which controls the size of the molecule or the average molecule for the case of mixed crystals

High-pressure behavior of CaMo O4

Science.gov (United States)

Panchal, V.; Garg, N.; Poswal, H. K.; Errandonea, D.; Rodríguez-Hernández, P.; Muñoz, A.; Cavalli, E.

2017-09-01

We report a high-pressure study of tetragonal scheelite-type CaMo O4 up to 29 GPa. In order to characterize its high-pressure behavior, we have combined Raman and optical-absorption measurements with density functional theory calculations. We have found evidence of a pressure-induced phase transition near 15 GPa. Experiments and calculations agree in assigning the high-pressure phase to a monoclinic fergusonite-type structure. The reported results are consistent with previous powder x-ray-diffraction experiments, but are in contradiction with the conclusions obtained from earlier Raman measurements, which support the existence of more than one phase transition in the pressure range covered by our studies. The observed scheelite-fergusonite transition induces significant changes in the electronic band gap and phonon spectrum of CaMo O4 . We have determined the pressure evolution of the band gap for the low- and high-pressure phases as well as the frequencies and pressure dependencies of the Raman-active and infrared-active modes. In addition, based on calculations of the phonon dispersion of the scheelite phase, carried out at a pressure higher than the transition pressure, we propose a possible mechanism for the reported phase transition. Furthermore, from the calculations we determined the pressure dependence of the unit-cell parameters and atomic positions of the different phases and their room-temperature equations of state. These results are compared with previous experiments showing a very good agreement. Finally, information on bond compressibility is reported and correlated with the macroscopic compressibility of CaMo O4 . The reported results are of interest for the many technological applications of this oxide.

K2SO4 and LiKSO4 crystals luminescence

International Nuclear Information System (INIS)

Charapiev, B.; Nurakhmetov, T.N.

2002-01-01

In the paper a nature of X-ray and tunnel luminescence in LiKSO 4 and Li 2 SO 4 ·H 2 O crystals are discussed. It is shown, that X-ray luminescence and Li 2 SO 4 ·H 2 O and LiKSO 4 appeals in the result of electrons recombination with auto-localized holes (SO 4 - ), and tunnel luminescence appeals at electrons transfer from ground state of electron center into hole center capture ground state. Under heating of irradiated crystal de-localized holes at recombination moment with electron capture centers are forming auto-localized excitons, which are disintegrating with photon emitting, and so X-ray luminescence spectrum and thermally induces luminescence peaks are coinciding. Nature of radiation appealing in LiKSO 4 at ultraviolet excitation is discussing

Faraday instability of crystallization waves in 4He

International Nuclear Information System (INIS)

Abe, H; Ueda, T; Morikawa, M; Saitoh, Y; Nomura, R; Okuda, Y

2007-01-01

Periodic modulation of the gravity acceleration makes a flat surface of a fluid unstable and standing waves are parametrically excited on the surface. This phenomenon is called Faraday instability. Since a crystal-superfluid interface of 4 He at low temperatures is very mobile and behaves like a fluid surface, Saarloos and Weeks predicted that Faraday instability of the crystallization waves exists in 4 He and that the threshold excitation for the instability depends on the crystal growth coefficient. We successfully observed the Faraday instability of the crystal-liquid interface at 160 mK. Faraday waves were parametrically generated at one half of the driving frequency 90 Hz. Amplitude of the Faraday wave becomes smaller at higher temperature due to decrease of the crystal growth coefficient and disappears above 200 mK

Crystal growth and luminescence properties of Pr-doped LuLiF4 single crystal

International Nuclear Information System (INIS)

Sugiyama, Makoto; Yanagida, Takayuki; Yokota, Yuui; Kurosawa, Shunsuke; Fujimoto, Yutaka; Yoshikawa, Akira

2013-01-01

0.1, 1, and 3% Pr (with respect to Lu) doped LuLiF 4 (Pr:LuLiF 4 ) single crystals were grown by the micro-pulling-down (μ-PD) method. Transparency of the grown crystals was higher than 70% in the visible wavelength region with some absorption bands due to Pr 3+ 4f-4f transitions. Intense absorption bands related with the Pr 3+ 4f-5d transitions were observed at 190 and 215 nm. In radioluminescence spectra, Pr 3+ 5d-4f emissions were observed at 220, 240, 340, and 405 nm. In the pulse height spectra recorded under 137 Cs γ-ray excitation, the Pr 3% doped sample showed the highest light yield of 2050 photons/MeV and the scintillation decay time of it exhibited 23 and 72 ns also excited by 137 Cs γ-ray. -- Highlights: ► 0.1, 1, and 3% Pr-doped LuLiF 4 single crystals were grown by the μ-PD method. ► Pr 3+ 5d-4f emission peaks appeared at 220, 240, 340, and 405 nm ► The Pr 3%:LuLiF 4 crystal showed the highest light yield of 2050 photons/MeV

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

Directory of Open Access Journals (Sweden)

Matthias Burgener

2016-05-01

Full Text Available 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.

Research on Cu2ZnSnTe4 crystals and heterojunctions based on such crystals

Directory of Open Access Journals (Sweden)

Kovaliuk T. T.

2015-12-01

Full Text Available The paper reports on the results of the studies of magnetic, kinetic and optical properties of Cu2ZnSnTe4 crystals. The Cu2ZnSnTe4 crystals showed diamagnetic properties (the magnetic susceptibility almost independent of the magnetic field and temperature. The Cu2ZnSnTe4 crystals possessed p-type of conductivity and the Hall coefficient was independent on temperature. The temperature dependence of the electrical conductivity of the Cu2ZnSnTe4 crystal shows metallic character, i. e. decreases with the increase of temperature, that is caused by the lower charge carrier mobility at higher temperature. Thermoelectric power of the samples ispositive that also indicates on the prevalence of p-type conductivity. Heterojunctions n-TiN/p-Cu2ZnSnTe4, n-TiO2/p-Cu2ZnSnTe4 and n-MoO/p-Cu2ZnSnTe4 were fabricated by the reactive magnetron sputtering of TiN, TiO2 and MoOx thin films, respectively, onto the substrates made of the Cu2ZnSnTe4 crystals. The dominating current transport mechanisms in the n-TiN/p-Cu2ZnSnTe4 and n-TiO2/p-Cu2ZnSnTe4 heterojunctions were established to be the tunnel-recombination mechanism at forward bias and tunneling at reverse bias.

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

Science.gov (United States)

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.

Optical absorption spectra of the uranium (4+) ion in the thorium germanate matrix

Energy Technology Data Exchange (ETDEWEB)

Gajek, Z. [W Trzebiatowski Institute of Low Temperature and Structure Research, Polish Academy of Sciences, 50-950 Wroclaw, PO Box 937 (Poland); Krupa, J.C. [Laboratoire de Radiochimie, Institut de Physique Nucleaire, BP 1, 91406 Orsay Cedex (France); Antic-Fidancev, E. [Unite P- de Recherche associee au CNRS 210, 1 place A Briand, 92195 Meudon Cedex (France)

1997-01-13

Visible and infrared absorption measurements on the U{sup 4+} ion in tetragonal zircon-type matrix {beta}-ThGeO{sub 4} are reported and analysed in terms of the standard parametrization scheme. The observed 17 main peaks and a number of less intense lines have been assigned and fitted to most of the 32 allowed electric dipole transitions with the root mean square error equal to 65 cm{sup -1}. The free-ion parameters obtained for the model Hamiltonian, {zeta}5f = 1809 cm{sup -1}, F{sup 2}=43 065 cm{sup -1}, F{sup 4}=38 977 cm{sup -1} and F{sup 6}=24 391 cm{sup -1}, as well as the corresponding crystal-field parameters, B{sub 0}{sup 2}=-1790 cm{sup -1}, B{sub 0}{sup 4}=1200 cm{sup -1}, B{sub 4}{sup 4}=3260 cm{sup -1}, B{sub 0}{sup 6}=-3170 cm{sup -1} and B{sub 4}{sup 6}=990 cm{sup -1}, agree fairly well with the initial theoretical estimations. The results are discussed in relation to the previous spectroscopic study on the scheelite-type matrix UGeO{sub 4}. (author)

Neutron single crystal diffraction studies of orientational glass state in the [Rbx(NH4)1-x]3H(SO4)2 mixed crystals

International Nuclear Information System (INIS)

Smirnov, L.S.; Reehuis, M.; Loose, A.; Hohlwein, D.; Hoffmann, J.U.; Wozniak, K.; Dominiak, P.; Baranov, A.I.; Dolbinina, V.V.

2005-01-01

The [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystal with the concentration x=0.0 at room temperature crystallizes in a monoclinic C2/c with sp.gr. (space group), which is stabilized for x>0.09 down to low temperatures. This system is transformed in the orientational glass state below the freezing temperature T g =30 K. The differential Fourier maps for the [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystals show that if for x=0.0 and 0.11 at 293 K the obtained maps reflect different orientational positions of crystallographically independent NH 4 (1) and NH 4 (2) groups, then the differential Fourier maps for x=0.20 at 9 K in the orientational glass state are similar for both ammonium groups reflecting their static disorder. The existence of the modulated structure in the [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystals with x=0.11 at 2 K is discovered, while the modulated structure for x=0.20 at 2 K is absent. This observation supposes that there should be two different regions of the orientational glass state on x-T phase diagram of the [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystals

The refractometry of the mechanically stressed RbNH4SO4 crystals

International Nuclear Information System (INIS)

Stadnik, V.J.; Romanyuk, M.O.

2001-01-01

The temperature (77-300K) and spectral (300-700hm) dependencies of refractive indices n i of mechanically unstressed and stressed by the pressures along general crystallophysic directions RbNH 4 SO 4 crystals were studied.the refractive indices were observed to decrease under pressure.The temperature and spectral dependencies of piezooptic constants were investigated.The changes of refraction,electron polarizability and the position of ultraviolet absorption effective center were calculated.The temperature and spectral dependencies of birefringence sign inversion of the mechanically unstressed and stressed RbNH 4 SO 4 crystals were analyzed

Electrical conduction studies in ferric-doped KHSO 4 single crystals

Science.gov (United States)

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.

Structure and stability of ZrSiO4 under hydrostatic pressure

DEFF Research Database (Denmark)

Marques, M.; Florez, M.; Recio, J.M.

2006-01-01

-anvil cell using energy-dispersive synchrotron x-ray diffraction with emphasis on the pressure range 0-15 GPa. Static total-energy calculations have been performed within the density functional theory at local density and generalized gradient approximation levels using a plane-wave pseudopotential scheme....... Our quantum-mechanical simulations explore the pressure response of the two observed tetragonal structures (zircon- and scheelite-type reidite) as well as of other potential post-scheelite polymorphs up to about 60 GPa. We find very good agreement between our experimental and calculated pressure......-volume values for the low-pressure phase of ZrSiO4. A microscopic analysis of the bulk compressibility of zircon and reidite in terms of polyhedral and atomic contributions is proposed to clarify some of the discrepancies found in recent theoretical and experimental studies. Our results show the relevant role...

A study on properties of PbWO4 crystal

International Nuclear Information System (INIS)

He Jingtang; Mao Yufang; Dong Xiaoli

1997-01-01

The experimental results on properties of the PbWO 4 crystal are reported, including the excitation and fluorescence spectra, absolute and relative light yield and decay times. It seems that the PbWO 4 crystal can be used in high energy physics experiments for detecting high energy shower particles

Crystallization of the FaeE chaperone of Escherichia coli F4 fimbriae

International Nuclear Information System (INIS)

Van Molle, Inge; Buts, Lieven; Coppens, Fanny; Qiang, Liu; Wyns, Lode; Loris, Remy; Bouckaert, Julie; De Greve, Henri

2005-01-01

The periplasmic chaperone FaeE of E. coli F4 fimbriae crystallizes in three crystal forms. F4 (formerly K88) fimbriae from enterotoxigenic Escherichia coli are assembled via the FaeE/FaeD chaperone/usher pathway. The chaperone FaeE crystallizes in three crystal forms, all belonging to space group C2. Crystals of form 1 diffract to 2.3 Å and have unit-cell parameters a = 195.7, b = 78.5, c = 184.6 Å, β = 102.2°. X-ray data for crystal form 2 were collected to 2.7 Å using an SeMet variant of FaeE. The crystals have unit-cell parameters a = 136.4, b = 75.7, c = 69.4 Å, β = 92.8°. Crystals of form 3 were formed in a solution containing the FaeE–FaeG complex and diffract to 2.8 Å. Unit-cell parameters are a = 109.7, b = 78.6, c = 87.8 Å, β = 96.4°

Crystallization of the FaeE chaperone of Escherichia coli F4 fimbriae

Energy Technology Data Exchange (ETDEWEB)

Van Molle, Inge, E-mail: ivmolle@vub.ac.be; Buts, Lieven; Coppens, Fanny; Qiang, Liu; Wyns, Lode; Loris, Remy; Bouckaert, Julie; De Greve, Henri [Laboratorium voor Ultrastructuur, Vlaams Interuniversitair Instituut voor Biotechnologie, Vrije Universiteit Brussel, Pleinlaan 2, 1050 Brussel (Belgium)

2005-04-01

The periplasmic chaperone FaeE of E. coli F4 fimbriae crystallizes in three crystal forms. F4 (formerly K88) fimbriae from enterotoxigenic Escherichia coli are assembled via the FaeE/FaeD chaperone/usher pathway. The chaperone FaeE crystallizes in three crystal forms, all belonging to space group C2. Crystals of form 1 diffract to 2.3 Å and have unit-cell parameters a = 195.7, b = 78.5, c = 184.6 Å, β = 102.2°. X-ray data for crystal form 2 were collected to 2.7 Å using an SeMet variant of FaeE. The crystals have unit-cell parameters a = 136.4, b = 75.7, c = 69.4 Å, β = 92.8°. Crystals of form 3 were formed in a solution containing the FaeE–FaeG complex and diffract to 2.8 Å. Unit-cell parameters are a = 109.7, b = 78.6, c = 87.8 Å, β = 96.4°.

Crystal structures of Er4Ni13C4 and UW4C4

International Nuclear Information System (INIS)

Khalili, M.M.; Bodak, O.I.; Marusin, E.P.; Pecharskaya, A.O.

1990-01-01

Crystal structures of Er 4 Ni 13 C 4 (1) (sp.gr. Cmmm, a=1.1975(4), b=1.1694(3), c=0.3856(1) nm, Z=2) and UW 4 C 4 (2) (sp.gr. P4/m, a=0.8328(8), c=0.31345(9) nm, Z=2), relating to new types are determined. Structural type (1) is a derivative of La 2 Ni 5 C 3 structure, structural type (2) is close to UCr 4 C 4 structure

Single crystal structures of the new vanadates CuMgVO{sub 4} and AgMgVO{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Ben Yahia, Hamdi, E-mail: Hyahia@qf.org.qa [Research Institute of Electrochemical Energy, National Institute of Advanced Industrial Science and Technology (AIST), 1-8-31 Midorigaoka, Ikeda, Osaka 563-8577 (Japan); Qatar Environment and Energy Research Institute, Hamad Bin Khalifa University, Qatar Foundation, PO Box 5825, Doha (Qatar); Shikano, Masahiro, E-mail: shikano.masahiro@aist.go.jp [Research Institute of Electrochemical Energy, National Institute of Advanced Industrial Science and Technology (AIST), 1-8-31 Midorigaoka, Ikeda, Osaka 563-8577 (Japan); Essehli, Rachid; Belharouak, Ilias [Qatar Environment and Energy Research Institute, Hamad Bin Khalifa University, Qatar Foundation, PO Box 5825, Doha (Qatar)

2016-08-01

The new compounds CuMgVO{sub 4} and AgMgVO{sub 4} have been synthesized by a solid state reaction route. Their crystal structures were determined from single-crystal X-ray diffraction data. CuMgVO{sub 4} crystallizes with Na{sub 2}CrO{sub 4}-type structure with space group Cmcm, a = 5.6932 (10), b = 8.7055 (15), c = 6.2789 (10) Å, V = 311.20 (9) Å{sup 3}, and Z = 4, whereas AgMgVO{sub 4} crystallizes in the maricite-type structure with space group Pnma, a = 9.4286 (14), b = 6.7465 (10), c = 5.3360 (8) Å, V = 339.42 (9) Å{sup 3}, and Z = 4. Both structures of CuMgVO{sub 4}, and AgMgVO{sub 4} contain MgO{sub 4} chains made up of edge-sharing MgO{sub 6} octahedra. In CuMgVO{sub 4} the MgO{sub 4} chains are interconnected through CuVO{sub 4} double chains made up of VO{sub 4} and CuO{sub 4} tetrahedra sharing corners and edges, however in AgMgVO{sub 4} the chains are interlinked by the VO{sub 4} and AgO{sub 4} tetrahedra sharing only corners. - Highlights: • We have been able to grow CuMgVO{sub 4} and AgMgVO{sub 4} single crystals. • We solved their crystal structures using single crystal data. • We compared the crystal structures of CuMgVO{sub 4} and AgMgVO{sub 4}.

Geology, mineralization, and fluid inclusion characteristics of the Kashkasu W-Mo-Cu skarn deposit associated with a high-potassic to shoshonitic igneous suite in Kyrgyzstan, Tien Shan: Toward a diversity of W mineralization in Central Asia

Science.gov (United States)

Soloviev, Serguei G.; Kryazhev, Sergey G.

2018-03-01

The Kashkasu deposit is part of the subduction-related Late Paleozoic (Late Carboniferous) metallogenic belt of Tien Shan. It is associated with a multiphase monzodiorite-monzonite-granodiorite-granite pluton of the magnetite-series high-K calc-alkaline to shoshonitic igneous suite. The deposit contains zones of W-Mo-Cu oxidized prograde and retrograde skarns, with abundant andraditic garnet, magnetite, locally scapolite and K-feldspar, as well as scheelite, chalcopyrite, and molybdenite. Skarns are overprinted by quartz-carbonate-sericite (phyllic alteration) zones with scheelite and sulfides. Prograde calcic skarn and initial retrograde skarns were formed from a high temperature (650 °C to 450-550 °C), high pressure (2000 bars to 600-900 bars) magmatic-hydrothermal low- to high-salinity aqueous chloride fluid. The gradual fluid evolution was interrupted by the intrusion of granodiorite and likely associated release of low-salinity (∼7-8 wt% NaCl equiv.) fluid. Ascent of this fluid to shallower levels and/or its cooling to 400-500 °C has resulted in phase separation into low-salinity (2.1-3.1 wt% NaCl equiv.) vapor and coexisting brine (35-40 wt% NaCl equiv.). The boiling was coincident with most intense scheelite deposition in retrograde skarn. Later retrograde skarn assemblages were formed from a gaseous, low- to moderate-salinity (3.4-8.1 wt% NaCl equiv.) fluid and then from high salinity (37-42 wt% NaCl equiv.) aqueous chloride fluids, the latter being enriched in Ca (17-20 wt% CaCl2) that could also affect scheelite deposition. Another cycle of fluid exsolution from crystallizing magma corresponded to quartz-carbonate-sericite-scheelite-sulfide (phyllic) alteration stage, with the early low-salinity (5.3-8.4 wt% NaCl-equiv.) fluid followed by later high-salinity (33.5-38.2 wt% NaCl-equiv.) fluid. The sulfur isotope data (δ34S = +5.1 to +9.0) suggest significant sulfur sourcing from sedimentary rocks enriched in seawater sulfate, possibly evaporites.

Crystal structure and dynamics of K2-x(NH4)xSeO4 mixed crystals studied by x-ray and neutron scattering

International Nuclear Information System (INIS)

Smirnov, L.S.; Natkaniec, I.; Loose, A.

2006-01-01

The K 2-x (NH 4 ) x SeO 4 mixed crystals have been studied by powder X-ray and neutron diffraction and inelastic incoherent neutron scattering in a wide temperature range from 300 to 16 K. No phase transition is observed in (NH 4 ) 2 SeO 4 in the range from room temperature to 20 K. The reorientation potential barriers of ammonium ions in the K 2-x (NH 4 ) x SeO 4 mixed crystals increase with the increasing concentration of ammonium ions

Crystal structure of PrRh4.8B2

International Nuclear Information System (INIS)

Higashi, Iwami; Shishido, Toetsu; Takei, Humihiko; Kobayashi, Takaaki

1988-01-01

The crystal structure of a new rare earth ternary boride PrRh 4.8 B 2 was investigated, by single-crystal X-ray diffractometry. PrRh 4.8 B 2 crystallizes in the orthorhombic space group Immm with a = 9.697(4), b = 5.577(2), c = 25.64(3) A, Z=12. The intensity data were collected on a four-circle diffractometer with graphite-monochromatized Mo Kα radiation. The structure was solved by the Patterson method and refined with a full-matrix least-squares program to an R value (equal to Σvertical strokeΔFvertical stroke/Σvertical strokeF 0 vertical stroke) of 0.055 for 1176 reflections. (orig.)

What is the reason for the doubled unit-cell volumes of copper-lead-rich pavonite homologues?

DEFF Research Database (Denmark)

Topa, Dan; Makovicky, Emil; Balic Zunic, Tonci

2008-01-01

The crystal Structure of cupromakovickyite, ideally Cu8Pb4Ag2Bi18S36, from the skarn deposit at Baita Bihor, in Romania, has been solved by direct methods and refined to an RI index of 5.36% for 2680 unique reflections measured with MOKU radiation oil it four-circle diffractometer equipped...... parameter for cupromakovickyite with respect to makovickyite. To be able to compare them, the crystal structure of Cu-bearing makovickyite, Cu2.25Ag1.56 (Pb0.27Cd0.13)(Sigma 0.4)Bi10.46S18, from a scheelite deposit at Felbertal, in Austria, has been refined to in R, index of 4.36% for 1320 unique...

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

Science.gov (United States)

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

Elastic properties of Ti-24Nb-4Zr-8Sn single crystals with bcc crystal structure

International Nuclear Information System (INIS)

Zhang, Y.W.; Li, S.J.; Obbard, E.G.; Wang, H.; Wang, S.C.; Hao, Y.L.; Yang, R.

2011-01-01

Research highlights: → The single crystals of Ti2448 alloy with the bcc crystal structure were prepared. → The elastic moduli and constants were measured by several resonant methods. → The crystal shows significant elastic asymmetry in tension and compression. → The crystal exhibits weak nonlinear elasticity with large elastic strain ∼2.5%. → The crystal has weak atomic interactions against crystal distortion to low symmetry. - Abstract: Single crystals of Ti2448 alloy (Ti-24Nb-4Zr-8Sn in wt.%) were grown successfully using an optical floating-zone furnace. Several kinds of resonant methods gave consistent Young's moduli of 27.1, 56.3 and 88.1 GPa and shear moduli of 34.8, 11.0 and 14.6 GPa for the , and oriented single crystals, and C 11 , C 12 and C 44 of 57.2, 36.1 and 35.9 GPa respectively. Uniaxial testing revealed asymmetrical elastic behaviors of the crystals: tension caused elastic softening with a large reversible strain of ∼4% and a stress plateau of ∼250 MPa, whereas compression resulted in gradual elastic stiffening with much smaller reversible strain. The crystals exhibited weak nonlinear elasticity with a large elastic strain of ∼2.5% and a high strength, approaching ∼20% and ∼30% of its ideal shear and ideal tensile strength respectively. The crystals showed linear elasticity with a small elastic strain of ∼1%. These elastic deformation characteristics have been interpreted in terms of weakened atomic interactions against crystal distortion to low crystal symmetry under external applied stresses. These results are consistent with the properties of polycrystalline Ti2448, including high strength, low elastic modulus, large recoverable strain and weak strengthening effect due to grain refinement.

Optical absorption spectra of the uranium (4+) ion in the thorium germanate matrix

CERN Document Server

Gajek, Z; Antic-Fidancev, E

1997-01-01

Visible and infrared absorption measurements on the U sup 4 sup + ion in tetragonal zircon-type matrix beta-ThGeO sub 4 are reported and analysed in terms of the standard parametrization scheme. The observed 17 main peaks and a number of less intense lines have been assigned and fitted to most of the 32 allowed electric dipole transitions with the root mean square error equal to 65 cm sup - sup 1. The free-ion parameters obtained for the model Hamiltonian, zeta 5f = 1809 cm sup - sup 1 , F sup 2 =43 065 cm sup - sup 1 , F sup 4 =38 977 cm sup - sup 1 and F sup 6 =24 391 cm sup - sup 1 , as well as the corresponding crystal-field parameters, B sub 0 sup 2 =-1790 cm sup - sup 1 , B sub 0 sup 4 =1200 cm sup - sup 1 , B sub 4 sup 4 =3260 cm sup - sup 1 , B sub 0 sup 6 =-3170 cm sup - sup 1 and B sub 4 sup 6 =990 cm sup - sup 1 , agree fairly well with the initial theoretical estimations. The results are discussed in relation to the previous spectroscopic study on the scheelite-type matrix UGeO sub 4. (author)

Comparative optical study of thulium-doped YVO4 , GdVO4 , and LuVO4 single crystals

Science.gov (United States)

Lisiecki, R.; Solarz, P.; Dominiak-Dzik, G.; Ryba-Romanowski, W.; Sobczyk, M.; Černý, Pavel; Šulc, Jan; Jelínková, Helena; Urata, Yoshiharu; Higuchi, Mikio

2006-07-01

YVO4:Tm3+ crystals grown by the Czochralski technique and GdVO4:Tm3+ and LuVO4:Tm3+ crystals grown by the floating-zone technique were investigated using methods of optical spectroscopy. Polarized absorption and emission spectra were recorded at room temperature and at 6K . The crystal-field analysis was performed assuming the D2d site symmetry for Tm3+ ions. In this way the missing crystal-field components of the H63 ground multiplet were located. Room temperature absorption spectra were analyzed in the framework of the Judd-Ofelt theory. Evaluated radiative lifetimes of luminescent levels of Tm3+ follow a general trend diminishing in agreement with the sequence: YVO4:Tm3+→GdVO4:Tm3+→LuVO4:Tm3+ . Luminescence lifetimes measured for the systems under study are similar except for the F43 lifetime, which appears to be surprisingly short for LuVO4:Tm3+ . Anisotropy of optical spectra is particularly pronounced in LuVO4:Tm3+ . Peak absorption cross section for the band relevant for optical pumping at about 805nm is roughly three times higher for π polarization. Stimulated emission cross sections for the F43-H63 transition near 1800nm were evaluated using the reciprocity method. The diode-pumped continuous wave laser operation in GdVO4:Tm3+ with a slope efficiency of up to 40% is demonstrated. In LuVO4:Tm3+ the diode-pumped laser oscillation in a pulsed mode was observed.

Crystal structure of 4-RbHo(PO3)4, 4-RbTm(PO3)4 and 4-CsEr(PO3)4

International Nuclear Information System (INIS)

Maksimova, S.I.; Palkina, K.K.; Chibiskova, N.T.

1982-01-01

X-ray structural study of 4-RbLn(PO 3 ) 4 (Ln=Mo, Tm) and 4-CsEr(PO 3 ) 4 is carried out. The compounds are crystallized in monoclinic crystal system, sp. gr P2 1 /n. Parameters of their unit cell, atom coordinates, anisotropic heat parameters, interatomic distances and valent angles are given. 4-RbHo(PO 3 ) 4 , 4-RbTm(PO 3 ) 4 , 4-CsEr(PO 3 ) 4 are isostructural to previously studied TlNd(PO 3 ) and 4-RbNd(PO 3 ) 4 . Using as an example the structural type 4-M 1 Ln(PO 3 ) 4 it is shown that the change of the shortest distances Ln-Ln, M 1 -M 1 and M 1 -Ln, as well as of degree of polymorphous chain corrugation to a higher extent depends on rare earth atom dimensions, than on monovalent metal ion dimensions [ru

Molecular and crystal structure of 3,4-dihydroxy-2-oxo-1-methyl-4-phenylpiperidine

International Nuclear Information System (INIS)

Kuleshova, L.N.; Khrustalev, V.N.; Struchkov, Yu.T.; Soldatenkov, A.T.; Bekro, I.A.; Mamyrbekova, Zh.A.; Soldatova, S.A.

1996-01-01

The molecular and crystal structure of 3,4-dihydroxy-2-oxo-1-methyl-4-phenylpiperidine was determined. The crystal is orthorhombic: sp. gr. Pca21; a=15.764, b=5.635, and c=25.536 A; and Z=8. The structure was solved by direct methods; R1=0.051, for 2643 unique refections. Symmetry-independent molecules are related by a pseudocenter of symmetry. The piperidine cycle has an asymmetric half-chair conformation. The orientation of substituents is determined. In the crystal, intermolecular OH...O hydrogen bonds link the molecules into chains parallel to the Y-axis

Preparation and crystal structure of Ca4Sb2O

International Nuclear Information System (INIS)

Eisenmann, B.; Limartha, H.; Schaefer, H.

1980-01-01

The formerly described compound Ca 2 Sb is to be corrected to Ca 4 Sb 2 O as shown by X-ray diffractometer data of single crystals and neutron diffraction diagrams of powders. The compound crystallizes in the K 2 NiF 4 structure type. (orig.)

Crystal growth, characterization and theoretical studies of 4-aminopyridinium picrate

Science.gov (United States)

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.

Crystal structures of two thiacalix[4]arene derivatives anchoring four ...

Indian Academy of Sciences (India)

Administrator

Abstract. The crystal structures of two thiacalixarene derivatives anchoring thiadiazole functional groups at lower rim, C60H72O4S12N8 (1), C64H80O4S12N8 (2), have been determined by single crystal X-ray diffraction. The thiacalix[4]arene framework in both 1 and 2 adopts the 1,3-alternate conformation. Com- pound 1 ...

A novel magneto-optical crystal Yb:TbVO4

Science.gov (United States)

Zhu, Xianchao; Tu, Heng; Hu, Zhanggui

2018-04-01

Highly transparent Yb:TbVO4 single crystal with dimensions of Ø27 × 41 mm3 alomost without scattering defects has been successfully grown by Czochralski technique. The spectra, thermal properties and laser-induced damage threshold were investigated in detailed. The Faraday rotation (FR) measurement was carried out by means of extinction method. The Verdet constant comes up to 80 rad m-1 T-1 at 1064 nm, significantly larger than TbVO4 (58 rad m-1 T-1) and TGG (40 rad m-1 T-1) reported. Meanwhile, the as-grown crystal presents lower absorption coefficient and higher magneto-optical figure of merit at measured wavelength in comparison with TGG. Moreover, the crystal exhibits a substantially improved extinction ratio (42 dB) in contrast with TbVO4 (29 dB), and exceeds the highest value of TGG (40 dB). These advantages make Yb:TbVO4 a highly promising magneto-optical material candidate for optical isolators in the visible-near infrared region.

X-ray and neutron single crystal diffraction on (NH4)3H(SO4)2. II. Refinement of crystal structure of phase II at room temperature

International Nuclear Information System (INIS)

Reehuis, M.; Wozniak, K.; Dominiak, P.; Smirnov, L.S.; Natkaniec, I.; Baranov, A.I.; Dolbinina, V.V.

2006-01-01

The (NH 4 ) 3 H(SO 4 ) 2 is of special interest due to the possible influence of ammonium ions on a series of phase transitions: I => II => III => IV => V => VII. Earlier, the X-ray single crystal diffraction study of phase II of (NH 4 ) 3 H(SO 4 ) 2 showed that the crystal structure of this compound has two crystallographically independent groups of ammonium ions NH 4 (1) and NH 4 (2), but orientational positions of these ammonium ions were not determined exactly. The refinement of NH 4 (1) and NH 4 (2) orientational positions in phase II is carried out with the help of the X-ray and neutron single crystal diffraction study. The analyses of differential Fourier maps of electron charge density and nuclear density point out the possibility of disordering of NH 4 (2) ammonium ions

Comparison of 2-Octanol and Tributyl Phosphate in Recovery of Tungsten from Sulfuric-Phosphoric Acid Leach Solution of Scheelite

Science.gov (United States)

Liao, Yulong; Zhao, Zhongwei

2018-04-01

Tungsten was recovered from sulfuric-phosphoric acid leach solution of scheelite using 2-octanol and tributyl phosphate (TBP). Approximately 76% of the tungsten and less than 6.2% of the iron were extracted when using 70% 2-octanol, showing good selectivity for tungsten over iron; the tungsten extraction could not be significantly enhanced using a three-stage countercurrent simulation test. Moreover, more than 99.2% of the W and 91.0% of the Fe were extracted when using 70% TBP, showing poor selectivity, but after pretreating the leach solution with iron powder, less than 5.5% of the Fe was extracted. The loaded phases were stripped using deionized water and ammonia solution. The maximum stripping rate of tungsten from loaded 2-octanol was 45.6% when using water, compared with only 13.1% from loaded TBP. Tungsten was efficiently stripped from loaded phases using ammonia solution without formation of Fe(OH)3 precipitate. Finally, a flow sheet for recovery of tungsten with TBP is proposed.

Time decay and photoluminescence measurement of PbWO4 crystal

International Nuclear Information System (INIS)

Baylac, M.

1997-09-01

This report presented the experimental characterization of the PbWO 4 crystals that we will be used for the photon detector of the Compton polarimeter at the Jefferson laboratory. We could draw 3 main features from this study. The transmission rate of the crystals is about 60 % in the scintillation wavelength region. From the decay time analysis, we deduced 3 decay components of the PbWO 4 , predicted by other measurements: τ 1 ∼5 ns, τ 2 ∼20 ns, τ 3 ∼100 ns, taking respectively 26 %, 30 % and 4 % of the total light amplitude emitted by the crystals. Moreover, we showed the existence of a fourth decay constant (τ 4 ∼1μs) taking 40 % of the total quantity of light which is responsible for the bad precision on the third constant determination. We could not characterize this component accurately because of the limited time range of the recordings. To improve the determination of the super-slow component, we need to perform the measurements again on a longer time scale, on the order of a few microseconds. We eventually measured the light yield of the PbWO 4 crystals. With a first analysis, we found about 3.5 photoelectrons per MeV whereas the constructors note gave about 10. We then reduced the light loss in the experimental set up by wrapping the last open end of the crystal. The results were slightly improved. Eventually, we increased the recording time, to take account the super-low decay, and found that the crystals yield about 6 photoelectrons per MeV which is still less than predicted. (author)

Crystal structure and characterization of the novel NH+⋯N hydrogen bonded polar crystal [NH2(CH2)4NH][BF4

International Nuclear Information System (INIS)

Wojtaś, M.; Gagor, A.; Czupiński, O.; Medycki, W.; Jakubas, R.

2012-01-01

Dielectric properties and phase transitions of the piperazinium tetrafluoroborate ([NH 2 (CH 2 ) 4 NH][BF 4 ], abbreviated as PFB) crystal are related to the one-dimensional arrangement of the cations linked by the bistable NH + ⋯N hydrogen bonds and molecular motions of the [BF 4 ] − units. The crystal structure of [NH 2 (CH 2 ) 4 NH][BF 4 ] is monoclinic at room temperature with the polar space group Pn. The polar/acentric properties of the room temperature phase IV have been confirmed by the piezoelectric and pyroelectric measurements. DSC measurements show that the compound undergoes three first-order structural phase transitions: at 421/411 K (heating/cooling), at 386/372 K and at 364/349 K. 1 H and 19 F NMR measurements indicate the reorientational motions of [BF 4 ] − anions and piperazinium(+) cations as well as the proton motion in the hydrogen-bonded chains of piperazine along the [001] direction. Over the phase I the isotropic reorientational motions or even self-diffusion of the cations and anions are expected. The conductivity measurements in the vicinity of the II–I PT indicate a superionic phase over the phase I. - Graphical abstract: It must be emphasized that the titled compound represents the first organic–inorganic simple salt containing the single-protonated piperazinium cation which was studied by means of the wide variety of experimental techniques. A survey of Cambridge Structural Database (CSD version 5.32 (November 2010) and updates (May 2011)) for structure containing the piperazinium cations yields 248 compounds with the doubly protonated piperazinium(2+) cations and only eight compounds with the singly protonated piperazinium(+) cations. Among these structures only one is the hybrid organic–inorganic material. This is piperazinium nitrate characterized structurally. The crystal packing of [NH 2 (CH 2 ) 4 NH][BF 4 ], phase IV. The dashed lines stand for the hydrogen bonds. The hydrogen bonds to BF4 groups are not included for

Crystal structure of (Al,V)4(P4O12)3, archetype of double cubic ring tetraphosphate

International Nuclear Information System (INIS)

Yakubovich, O. V.; Biralo, G. V.; Dimitrova, O. V.

2012-01-01

The crystal structure of the (Al,V) 4 (P 4 O 12 ) 3 solid solution, obtained in the single-crystal form by hydrothermal synthesis in the Al(OH) 3 -VO 2 -NaCl-H 3 PO 4 -H 2 O system, has been solved by X-ray diffraction analysis (Xcalibur-S-CCD diffractometer, R = 0.0257): a = 13.7477(2) Å, sp. gr. I 4 bar 3d, Z = 4, and ρ calcd = 2.736 g/cm 3 . It is shown that the crystal structure of the parent cubic Al 4 (P 4 O 12 ) 3 modification can formally be considered an archetype for the formation of double isosymmetric tetraphosphates on its basis.

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

Science.gov (United States)

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.

Crystal structures of 4-meth-oxy-N-(4-methyl-phenyl)benzene-sulfonamide and N-(4-fluoro-phenyl)-4-meth-oxy-benzene-sulfonamide.

Science.gov (United States)

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.

Polarized spectral properties of Sm3+:LiYF4 crystal

International Nuclear Information System (INIS)

Wang, G.Q.; Lin, Y.F.; Gong, X.H.; Chen, Y.J.; Huang, J.H.; Luo, Z.D.; Huang, Y.D.

2014-01-01

A trivalent samarium-doped LiYF 4 single crystal was grown by the vertical Bridgman technique. Its polarized absorption and fluorescence spectra and fluorescence decay curves were recorded at room temperature. On the basis of the Judd–Ofelt theory, the spectral parameters of the Sm 3+ :LiYF 4 crystal were calculated. The emission cross sections for the 4 G 5/2 → 6 H J (J=5/2, 7/2. 9/2, and 11/2) transitions of special interest for visible laser application were obtained by the Fuchtbauer–Ladenburg formula. -- Highlights: • Polarized spectral properties of Sm 3+ :LiYF 4 crystal at room temperature were analyzed in detail. • The emission cross sections for the transitions of special interest for visible laser application are calculated. • Sm 3+ :LiYF 4 is a promising laser material for 401 nm GaN LD pumped 605 nm visible laser

Non-uniformity measurements of PbWO4 crystals

International Nuclear Information System (INIS)

Depasse, P.; Ernenwein, J.P.; Ille, B.; Martin, F.; Rosset, C.; Zach, F.

1998-11-01

Two independent methods have been used to measure the longitudinal non-uniformity scintillation response of 3 different (23-cm long) PbWO 4 crystals. The first one is the classical 60 Co source method. The source is collimated along the crystal, each 1,5-cm, and the scintillation signal is measured with a photomultiplier (a hybrid photomultiplier in our case). The second one is the use of cosmic particles (Minimum Ionizing Particles). A cosmic bench allows reconstructing the track of the MIP's and thus the energy deposit with the help of a full GEANT simulation of the setup. Variations of E along the crystal artificially cut in 1,5-cm divisions, leads to determine the non-uniformity. The conclusion is that both methods agree quite well. Furthermore, a good estimation of crystal light yield can be obtained. (author)

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

Science.gov (United States)

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.

PAK4 crystal structures suggest unusual kinase conformational movements.

Science.gov (United States)

Zhang, Eric Y; Ha, Byung Hak; Boggon, Titus J

2018-02-01

In order for protein kinases to exchange nucleotide they must open and close their catalytic cleft. These motions are associated with rotations of the N-lobe, predominantly around the 'hinge region'. We conducted an analysis of 28 crystal structures of the serine-threonine kinase, p21-activated kinase 4 (PAK4), including three newly determined structures in complex with staurosporine, FRAX486, and fasudil (HA-1077). We find an unusual motion between the N-lobe and C-lobe of PAK4 that manifests as a partial unwinding of helix αC. Principal component analysis of the crystal structures rationalizes these movements into three major states, and analysis of the kinase hydrophobic spines indicates concerted movements that create an accessible back pocket cavity. The conformational changes that we observe for PAK4 differ from previous descriptions of kinase motions, and although we observe these differences in crystal structures there is the possibility that the movements observed may suggest a diversity of kinase conformational changes associated with regulation. Protein kinases are key signaling proteins, and are important drug targets, therefore understanding their regulation is important for both basic research and clinical points of view. In this study, we observe unusual conformational 'hinging' for protein kinases. Hinging, the opening and closing of the kinase sub-domains to allow nucleotide binding and release, is critical for proper kinase regulation and for targeted drug discovery. We determine new crystal structures of PAK4, an important Rho-effector kinase, and conduct analyses of these and previously determined structures. We find that PAK4 crystal structures can be classified into specific conformational groups, and that these groups are associated with previously unobserved hinging motions and an unusual conformation for the kinase hydrophobic core. Our findings therefore indicate that there may be a diversity of kinase hinging motions, and that these may

Infrared-active optical phonons in LiFePO4 single crystals

Science.gov (United States)

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.

Spectroscopy of V4+ and V3+ ions in a forsterite crystal

International Nuclear Information System (INIS)

Veremeichik, T F; Gaister, A V; Subbotin, Kirill A; Zharikov, Evgeny V; Protopopov, V N; Smirnov, Valerii A

2000-01-01

The absorption spectra of impurity vanadium ions in forsterite crystals are studied in the wavelength range from 600 to 2000 nm. It is found that the V 4+ ion in the tetrahedral coordination in crystals grown by the Czochralski technique exhibits strong absorption in the range from 600 to 1200 nm. The intense electron-vibrational progressions in the absorption spectra of impurity d-ions in crystals were observed for the first time at temperatures 300 and 77 K. In the authors' opinion, these progressions appear due to the formation of the oxovanadate complex and distortions of the structural tetrahedron. The forsterite crystal doped with V 4+ ions has a very high absorption cross section (up to 2.1x10 -18 cm 2 ) and a continuous broad absorption band, which makes this crystal promising as a passive laser switch in the range between 600 and 1200 nm. At the same time, the V 4+ ions in the forsterite crystal do not emit luminescence because of a high probability of the nonradiative relaxation of their excited state. It is shown that luminescence of a V:Mg 2 SiO 4 crystal is related to the tetrahedral V 3+ ion. (laser applications and other topics in quantum electronics)

Magnetic SiO2/Fe3O4 colloidal crystals

International Nuclear Information System (INIS)

Huang, C-K; Hou, C-H; Chen, C-C; Tsai, Y-L; Chang, L-M; Wei, H-S; Hsieh, K-H; Chan, C-H

2008-01-01

We proposed a novel technique to fabricate colloidal crystals by using monodisperse SiO 2 coated magnetic Fe 3 O 4 (SiO 2 /Fe 3 O 4 ) microspheres. The magnetic SiO 2 /Fe 3 O 4 microspheres with a diameter of 700 nm were synthesized in the basic condition with ferric sulfate, ferrous sulfate, tartaric acid and tetraethyl orthosilicate (TEOS) in the reaction system. Monodisperse SiO 2 /Fe 3 O 4 superparamagnetic microspheres have been successfully used to fabricate colloidal crystals under the existing magnetic field

Hydrothermal growth of PbSO4 (Anglesite) single crystal

International Nuclear Information System (INIS)

Kikuta, Ko-ichi; Yoneta, Yasuhito; Yogo, Toshinobu; Hirano, Shin-ichi

1994-01-01

Hydrothermal growth of single crystals of PbSO 4 , which is known as a natural mineral called anglesite, was investigated. Lead nitrate and nitric acid solutions were found to be useful for the growth of angle-site on the basis of the experimental results on the dissolution behavior. Relatively large euhedral single crystals bound by {210} and {101} planes were successfully grown in 1.5 mol/kg Pb(NO 3 ) 2 at 400degC and 100 MPa. Optical characterization revealed that the grown anglesite crystals can be useful for scintillators material. (author)

Crystal growth and optical properties of 4-aminobenzophenone (ABP)

Science.gov (United States)

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.

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

Science.gov (United States)

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.

Annealing effect on superconductivity of La2CuO4 single crystals

International Nuclear Information System (INIS)

Tanaka, I.; Takahashi, H.; Kojima, H.

1992-01-01

This paper reports that La 2 CuO 4 single crystals grown at an oxygen pressure of 0.2 MPa by TSFZ method are superconducting below 32 K, and show a semiconducting behavior in nonsuperconducting state. The single crystals of La 2 CuO 4 are changed from superconductors to semiconductors by annealing in argon, and are returned to superconductors by annealing at ambient pressure of oxygen. Therefore, superconductivity of the La 2 CuO 4 single crystals is due to excess oxygen

Annealing effect on superconductivity of La2CuO4 single crystals

International Nuclear Information System (INIS)

Tanaka, L.; Takahashi, H.; Kojima, H.

1992-01-01

La 2 CuO 4 single crystals grown at an oxygen pressure of 0.2 MPa by TSFZ method are superconducting below 32 K, and show a semiconducting behavior in nonsuperconducting state. The single crystals of La 2 CuO 4 are changed from superconductors to semiconductors by annealing in argon, and are returned to superconductors by annealing at ambient pressure of oxygen. Therefore, superconductivity of the La 2 CuO 4 single crystals is due to excess oxygen. (orig.)

Synthesis and thermophysical properties of AMoO4 (A = Ca, Sr, Ba)

International Nuclear Information System (INIS)

Maji, Binoy Kumar; Jena, Hrudananda; Asuvathraman, R.; Govindan Kutty, K.V.

2013-01-01

The alkaline earth molybdates AMoO 4 (A=Ca, Sr, Ba) belong to Scheelite type crystal structure with space group 14 1 /a, and are naturally occurring minerals. They are often found as secondary phases in irradiated oxide nuclear fuels as a product of fission product interaction. These compounds can also form as microcrystallites when the high-level nuclear waste is vitrified. As high temperature ceramics, they find applications as sensor materials, oxide ion conductors, etc. The thermophysical properties of these molybdates are essential for understanding their impact on the high temperature properties of the systems and devices containing them. In the present study, these compounds were synthesized by solid state reaction route in air at 823 K, and characterized by powder XRD and TG/DTA. The thermal expansion behavior was investigated by dilatometry in the temperature range of 300-800 K in air. The % thermal expansion of BaMoO 4 was found to be the lowest among the three compounds. The electrical conductivity of the compounds was measured by AC-impedance spectroscopy, and the conductivity was found to be in the range of 10 -4 S.cm -1 at 1073 K in air. The activation energy of electrical conduction was measured to be about 1.3 eV. (author)

Polymorphism of felodipine co-crystals with 4,4'-bipyridine

DEFF Research Database (Denmark)

Surov, Artem Olegovich; Solanko, Katarzyna A.; Bond, Andrew

2014-01-01

-crystal is the most thermodynamically stable phase. The difference in the crystal lattice energies between different polymorphs of the co-crystal is found to be comparable with that between the polymorphic forms of pure felodipine. The enthalpies of formation of the co-crystals are small, which indicates...

Optical and scintillating properties of Ce:Li(Y,Lu)F4 single crystals

International Nuclear Information System (INIS)

Yokota, Yuui; Kurosawa, Shunsuke; Chani, Valery; Kamada, Kei; Yoshikawa, Akira

2014-01-01

We have investigated the optical and scintillating properties of Lu co-doped Ce:LiYF 4 single crystals with various Lu content. In the transmittance and absorption spectra, the absorption peaks at 243 nm get systematically red shifted in contrast to the peaks at 197 and 200 nm which get blue shifted with the increase in Lu content. At the same time, emission peaks at 306 nm and 200 nm under 295 nm excitation also get red shifted. The decay time of Ce:Li(Y,Lu)F 4 crystals under 295 nm excitation is found to be faster than that of Ce:LiYF 4 and Ce:LiLuF 4 crystals. The alpha-peak positions in the pulse-height spectra and decay times of crystals under alpha-ray irradiation are found to vary with the Lu content. - Highlights: • Optical and scintillation properties of Ce:Li(Y 1-x Lu x )F 4 crystals were inspected. • Increase of Lu content resulted change of the position of four absorption peaks. • Admixing of Y and Lu decreased the light yield and increased the decay time. • The Ce:LiLuF 4 crystal indicated the largest light yield in the pulse-height spectra. • Li[(Y 0.8 Lu 0.2 ) 0.98 Ce 0.02 ]F 4 indicated larger light yield than Ce:LiYF 4 crystal

X-ray and neutron single-crystal diffraction on [Rbx(NH4)1-x]3H(SO4)2. I. Refinement of crystal structure of phase II with x=0.11 at 300 K

International Nuclear Information System (INIS)

Loose, A.; Wozniak, K.; Dominiak, P.; Smirnov, L.S.; Natkaniec, I.; Frontas'eva, M.V.; Pomyakushina, E.V.; Baranov, A.I.; Dolbinina, V.V

2006-01-01

The study of [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystals by X-ray single-crystal diffraction is known up to now only for x=0.57 at the temperatures 293 and 180 K. The crystal structures at these temperatures as was determined [1] belong to monoclinic phase II (C2/c sp. gr., Z=4). In accordance with this work, ammonium ions should be considered as deformed tetrahedra. Monoclinic phase II on the x-T phase diagram of [Rb x (NH 4 ) 1-x ] 3 H(SO 4 ) 2 mixed crystals, which has earlier been determined by the dielectric spectroscopy, is stabilized below room temperature if Rb concentration exceeds 9%. The presented results of X-ray and neutron single-crystal diffraction of the [Rb 0.11 (NH 4 ) 0.89 ] 3 H(SO 4 ) 2 mixed crystal at T= 300 K show that ammonium ions could be considered as regular tetrahedra

Crystal structure of (E-4,4,4-trifluoro-3-phenylbut-2-enoic acid

Directory of Open Access Journals (Sweden)

Alexey Barkov

2015-12-01

Full Text Available In the title compound, C10H7F3O2, the dihedral angle between the benzene ring and the ethylene plane is 76.34 (11°. In the crystal, O—H...O hydrogen bonds link the molecules into C(4 chains propagating in [010].

Crystal Structure of Tetragonal Form of La2NiO4+x

Science.gov (United States)

Kajitani, Tsuyoshi; Hosoya, Syoichi; Hirabayashi, Makoto; Fukuda, Tsuguo; Onozuka, Takashi

1989-10-01

The crystal structure of the title oxide was studied by means of the X-ray and neutron single crystal diffraction measurements. At room temperature, the tetragonal crystal structure is P42/ncm-type (No. 138), which is one of the subgroup of the space group I4/mmm. The lattice parameters of a sample annealed and slowly cooled in oxygen atmosphere from 673 K are a{=}b{=}5.4640(1) Å and c{=}12.6719(2) Å, while the oxygen content, x{=}0.10(4), was determined from obtained neutron data. The title oxide undergoes a tetragonal (P42/ncm)/tetragonal (I4/mmm) phase transition at about 560 K. The transition temperature is almost identical both in the annealed and as-grown crystals.

Crystal structure of the Hg4SiS6 and Hg4SiSe6 compounds

International Nuclear Information System (INIS)

Gulay, L.D.; Olekseyuk, I.D.; Parasyuk, O.V.

2002-01-01

The crystal structures of Hg 4 SiS 6 and Hg 4 SiSe 6 compounds were investigated using X-ray powder diffraction. These compounds crystallize in the monoclinic Cc space group with the lattice parameters a=1.23020(5), b=0.71031(4), c=1.22791(4) nm, β=109.721(3) deg. for Hg 4 SiS 6 and a=1.28110(4), b=0.74034(4), c=1.27471(1) nm, β=109.605(3) deg. for Hg 4 SiSe 6 . Atomic parameters were refined in the isotropic approximation (R I =0.0571 and R I =0.0555 for the Hg 4 SiS 6 and Hg 4 SiSe 6 , respectively)

Phase transitions in (NH4)2MoO2F4 crystal

Science.gov (United States)

Krylov, Alexander; Laptash, Natalia; Vtyurin, Alexander; Krylova, Svetlana

2016-11-01

The mechanisms of temperature and high pressure phase transitions have been studied by Raman spectroscopy. Room temperature (295 K) experiments under high hydrostatic pressure up to 3.6 GPa for (NH4)2 MoO2 F4 have been carried out. Experimental data indicates a phase transition into a new high-pressure phase for (NH4)2 MoO2 F4 at 1.2 GPa. This phase transition is related to the ordering anion octahedron groups [MoO2 F4]2- and is not associated with ammonium group. Raman spectra of small non-oriented crystals ranging from 10 to 350 K have been observed. The experiment shows anion groups [MoO2 F4]2- and ammonium in high temperature phase are disordered. The phase transition at T1 = 269.8 K is of the first-order, close to the tricritical point. The first temperature phase transition is related to the ordering anion octahedron groups [MoO2 F4]2-. Second phase transitions T2 = 180 K are associated with the ordering of ammonium. The data presented within this study demonstrate that 2D correlation analysis combined with traditional Raman spectroscopy are powerful tool to study phase transitions in the crystals.

Fergusonite-type CeNbO{sub 4+δ}: Single crystal growth, symmetry revision and conductivity

Energy Technology Data Exchange (ETDEWEB)

Bayliss, Ryan D. [Department of Materials, Imperial College London, Prince Consort Road, London, SW7 2BP (United Kingdom); Pramana, Stevin S.; An, Tao; Wei, Fengxia; Kloc, Christian L. [School of Materials Science and Engineering, 50 Nanyang Avenue, Nanyang Technological University, 639798 (Singapore); White, Andrew J.P. [Chemical Crystallography Laboratory, Department of Chemistry, Imperial College London, Exhibition Road, London, SW7 2AZ (United Kingdom); Skinner, Stephen J. [Department of Materials, Imperial College London, Prince Consort Road, London, SW7 2BP (United Kingdom); White, Timothy J. [School of Materials Science and Engineering, 50 Nanyang Avenue, Nanyang Technological University, 639798 (Singapore); Baikie, Tom, E-mail: tbaikie@ntu.edu.sg [School of Materials Science and Engineering, 50 Nanyang Avenue, Nanyang Technological University, 639798 (Singapore)

2013-08-15

Large fergusonite-type (ABO{sub 4}, A=Ce, B=Nb) oxide crystals, a prototype electrolyte composition for solid oxide fuel cells (SOFC), were prepared for the first time in a floating zone mirror furnace under air or argon atmospheres. While CeNbO{sub 4} grown in air contained CeNbO{sub 4.08} as a minor impurity that compromised structural analysis, the argon atmosphere yielded a single phase crystal of monoclinic CeNbO{sub 4}, as confirmed by selected area electron diffraction, powder and single crystal X-ray diffraction. The structure was determined in the standard space group setting C12/c1 (No. 15), rather than the commonly adopted I12/a1. AC impedance spectroscopy conducted under argon found that stoichiometric CeNbO{sub 4} single crystals showed lower conductivity compared to CeNbO{sub 4+δ} confirming interstitial oxygen can penetrate through fergusonite and is responsible for the higher conductivity associated with these oxides. - Graphical abstract: Large fergusonite-type CeNbO{sub 4} crystals were prepared for the first time in a floating zone mirror furnace. Crystal growth in an argon atmosphere yielded a single phase monoclinic CeNbO4, as confirmed by selected area electron diffraction, powder and single crystal X-ray diffraction. The structure was determined in the standard space group setting C12/c1 (No. 15), rather than the commonly adopted I12/a1. AC impedance spectroscopy found CeNbO{sub 4} single crystals showed lower conductivity compared to CeNbO{sub 4+δ} confirming interstitial oxygen can penetrate through fergusonite and is responsible for the higher conductivity associated with these oxides. Highlights: • Preparation of single crystals of CeNbO{sub 4} using a floating zone mirror furnace. • Correction to the crystal symmetry of the monoclinic form of CeNbO{sub 4}. • Report the conductivity of a single crystal of CeNbO{sub 4}.

Spectroscopic and crystallographic studies of YAG:Pr4+ single crystals

International Nuclear Information System (INIS)

Pawlak, D.; Frukacz, Z.; Mierczyk, Z.; Suchocki, A.; Zachara, J.

1998-01-01

Y 3 Al 5 O 12 single crystals doped with praseodymium and magnesium ions have been prepared. The reversible color change of this crystal is observed when annealing in oxidizing or reducing atmospheres. The change is ascribed to the formation of Pr 4+ in the as-grown crystal, caused by the second dopant, Mg 2+ . The absorption spectra of YAG:Pr,Mg in the range 200-1100 nm, as grown and annealed in air and H 2 /N 2 atmosphere, are presented and discussed. Additional broad absorption bands are observed for the as-grown crystals and those annealed in oxidizing atmosphere. Crystallographic investigations of the original crystal and after annealing in a reducing atmosphere as described above, show no distinct structural differences. A redox mechanism is proposed to explain the color change during annealing. (orig.)

Growth of NH4Cl Single Crystal from Vapor Phase in Vertical Furnace

Science.gov (United States)

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.

Optical characteristics of BaGa2S4:Ho3+ and BaGa2Se4:Ho3+ single crystals

International Nuclear Information System (INIS)

Choe, Sung-Hyu; Jin, Moon-Seog; Kim, Wha-Tek

2005-01-01

BaGa 2 S 4 , BaGa 2 S 4 :Ho 3+ , BaGa 2 Se 4 , and BaGa 2 Se 4 :Ho 3+ single crystals were grown by using the chemical transport reaction method. The optical energy gaps of the single crystals were investigated in the temperature region from 11 K to 300 K. The temperature dependence of the optical energy gap was well fitted by the Varshni equation. Two broad emission bands were observed in the photoluminescence spectra of the single crystals. These bands were attributed to donor-acceptor pair recombinations. Sharp emission peaks were observed in the BaGa 2 S 4 :Ho 3+ and the BaGa 2 Se 4 :Ho 3+ single crystals and were assigned to radiation recombination between split Stark levels of Ho 3+ .

Production of CaWO{sub 4} crystals for direct dark matter search with CRESST

Energy Technology Data Exchange (ETDEWEB)

Muenster, Andrea [Physik-Department and Excellence Cluster Universe, Technische Universitaet Muenchen, D-85748 Garching (Germany); Collaboration: CRESST-Collaboration

2016-07-01

The direct dark matter search experiment CRESST (Cryogenic Rare Event Search with Superconducting Thermometers) uses scintillating CaWO{sub 4} single crystals as targets for possible recoils of dark matter particles. Since several years these CaWO{sub 4} crystals are produced directly at the Technische Universitaet Muenchen (TUM) including the CaWO{sub 4} powder production from the raw materials CaCO{sub 3} and WO{sub 3}, the CaWO{sub 4} crystal growth via the Czochralski method as well as the after-growth treatment of the crystals. In the recently finished CRESST-II Phase 2 (2013-2015), 4 TUM-grown crystals were installed in the main cryostat for the first time. Showing one of the best radiopurities of all installed crystals combined with an excellent detector performance the analysis of the crystal TUM40 resulted in the best sensitivity for low-mass dark matter particles in 2014. For the upcoming CRESST-III phase 2 we aim for a further improvement in radiopurity by a factor of 100. First results of a chemical purification of the raw materials as well as future plans to reduce the intrinsic background via recrystallization are presented.

Synthesis and crystal structure of the cesium silver permanganate Cs_3Ag[MnO_4]_4

International Nuclear Information System (INIS)

Bauchert, Joerg M.; Henning, Harald; Schleid, Thomas

2012-01-01

After successful syntheses and structural refinements of the already known permanganates of cesium (Cs[MnO_4]) and silver (Ag[MnO_4]) we started to blend aqueous solutions of both components in various molar ratios. From crystallization experiments of these mixtures only three species of crystals with different chemical compositions were obtained: tricesium monosilver tetrakispermanganate (Cs_3Ag[MnO_4]_4) and, depending upon the respective ratio, either additional silver permanganate or surplus cesium permanganate, namely. The new title compound crystallizes in the orthorhombic space group Pnnm (no. 58) with two formula units per unit cell and cell dimensions of a = 764.53(4), b = 1883.57(9) and c = 584.34(3) pm. The crystal structure of Cs_3Ag[MnO_4]_4 consists of two crystallographically distinguishable cesium cations. (Cs1)"+ is surrounded by fourteen oxygen atoms constructing a slightly distorted bicapped hexagonal prism. These polyhedra are connected through edge-sharing with two other polyhedra of this kind to form chains along [001]. The chains are linked to each other via sixfold coordinated Ag"+ cations (d(Ag-O) = 238-246 pm), arranged in such a manner that they link three oxygen atoms of two cesium polyhedra, leading to a two-dimensional layer spreading out parallel to the (001) plane. Together with the two crystallographically different tetrahedral oxomanganate(VII) anions [MnO_4]"- (d(Mn-O) = 161-162 pm) the other kind of cesium cations ((Cs2)"+ with CN = 13) finally connect these layers three-dimensionally. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Crystal structures and conformers of CyMe4-BTBP

Directory of Open Access Journals (Sweden)

Lyczko Krzysztof

2015-12-01

Full Text Available The crystal structure of new conformation of the CyMe4-BTBP ligand (ttc has been presented. The ttt conformer of this compound in a form of THF solvate has been also crystallized. The geometries of six possible conformations (ttt, ttc, tct, tcc, ctc and ccc of the CyMe4-BTBP ligand have been modeled in the gas phase and in solutions (MeOH and H2O by DFT calculations using B3LYP/6-31G(d,p method. According to the calculations, in the three different media the conformers with trans orientation of the N atoms in the bipyridyl moiety are the most stable.

Crystal structure and crystal growth of the polar ferrimagnet CaBaFe4O7

Science.gov (United States)

Perry, R. S.; Kurebayashi, H.; Gibbs, A.; Gutmann, M. J.

2018-05-01

Magnetic materials are a cornerstone for developing spintronic devices for the transport of information via magnetic excitations. To date, relatively few materials have been investigated for the purpose of spin transport, mostly due to the paucity of suitable candidates as these materials are often chemically complex and difficult to synthesize. We present the crystal growth and a structure solution on the high-temperature crystal structure of the layered, polar ferrimagnet CaBaFe4O7 , which is a possible new contender for spintronics research. The space group is identified as P 3 by refinement of single crystal and powder neutron diffraction data. At 400 K, the trigonal lattice parameters are a =11.0114 (11 )Å and c =10.330 (3 )Å . The structure is similar to the low-temperature phase with alternating layers of triangular and Kagome-arranged Fe-O tetrahedra. We also present details of the crystal growth by traveling solvent method.

Preparation and characterisation of radiation hard PbWO4 crystal scintillator

International Nuclear Information System (INIS)

Sabharwal, S.C.; Desai, D.G.; Sangeeta; Karandikar, S.C.; Chauhan, A.K.; Sangiri, A.K.; Keshwani, K.S.; Ahuja, M.N.

1996-01-01

The selective loss of one of the crystal constituents is found to be responsible for the yellowish coloration of PbWO 4 crystals. However, using the already pulled crystals as the starting charge for the subsequent growth, colorless crystals can be grown. The crystals exhibiting excellent transmission characteristics have been grown employing a low temperature gradient, a moderate rotation rate of 15 rpm and a pull speed of 1 mm/h. The colored crystals show some radiation damage on gamma irradiation, while the colorless ones remain unaffected even for irradiation doses as high as 10 Mrad. Both the types of crystals show the presence of weak thermoluminescence (TL) emission when high irradiation doses (similar 10 Mrad) are given. Only one TL glow peak is obtained in both the cases but the peak temperatures are different. The emission centers responsible for the TL emission are found to be the ones which give rise to the scintillation emission in the crystal. (orig.)

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

Science.gov (United States)

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}.

Scintillation properties of pure and Ca-doped ZnWO4 crystals

International Nuclear Information System (INIS)

Danevich, F.A.; Shkulkova, O.G.; Henry, S.; Kraus, H.; McGowan, R.; Mikhailik, V.B.; Telfer, J.

2008-01-01

Following the investigations of the structure and scintillation properties of Ca-doped zinc tungstate powder [phys. stat. sol. (a) 204, 730 (2007)] a single-crystal of ZnWO 4 -Ca (0.5 mol%) was grown and characterised. The relative light output, energy resolution and decay characteristics were measured for pure and Ca-doped ZnWO 4 scintillators. An increase in the light yield of ∝40% compared with the undoped crystal, and an energy resolution 9.6% ( 137 Cs) were obtained for Ca-doped ZnWO 4 . The observed improvement is attributed to the reduction of self-absorption (bleaching) of the crystal. The cause of bleaching as well as the possible contribution of scattering is discussed. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Radiation defects in SrB4O7:Eu2+ crystals

International Nuclear Information System (INIS)

Yavetskiy, R.P.; Dolzhenkova, E.F.; Tolmachev, A.V.; Parkhomenko, S.V.; Baumer, V.N.; Prosvirnin, A.L.

2007-01-01

Radiation-induced defects in SrB 4 O 7 :Eu 2+ (0.033 at.%) single crystal irradiated with γ and X-ray quanta has been studied. The induced optical absorption in the 400-700 nm region has been ascribed to F + centers. The Eu 2+ ions have been shown to act simultaneously as traps and as radiative recombination centers of charge carriers. Basing on the thermally stimulated luminescence (TSL), optical absorption and photoluminescence studies of SrB 4 O 7 :Eu 2+ crystals, a TSL mechanism has been proposed associated with the decay of F + centers being in non-equivalent crystallographic positions followed by radiative recombination of charge carriers on europium ions. Various positions of localization of the radiation-induced defects in the SrB 4 O 7 crystal structure have been discussed

Preparation and crystal structure of Ca/sub 4/Sb/sub 2/O

Energy Technology Data Exchange (ETDEWEB)

Eisenmann, B; Limartha, H; Schaefer, H; Graf, H A

1980-12-01

The formerly described compound Ca/sub 2/Sb is to be corrected to Ca/sub 4/Sb/sub 2/O as shown by X-ray diffractometer data of single crystals and neutron diffraction diagrams of powders. The compound crystallizes in the K/sub 2/NiF/sub 4/ type structure.

Study on light output and energy resolution of PbWO4 crystal

International Nuclear Information System (INIS)

Su Guanghui; Yue Ke; Sun Zhiyu

2010-01-01

The light output and energy resolution of PbWO 4 crystal are studied with different wrapping materials and methods. The Wrapping condition was optimized by analyzing the experimental data to gain higher light output and better energy resolution. A GEANT4-based package has been developed to simulate the corresponding features of PbWO 4 crystal, and the simulation results are consistent with the experimental data. (authors)

Crystal growth, defects, and mechanical and spectral properties of a novel mixed laser crystal Nd:GdYNbO{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Ding, Shoujun; Dou, Renqin [Chinese Academy of Sciences, Anhui Institute of Optics and Fine Mechanics, Hefei, Anhui Province (China); University of Science and Technology of China, Hefei (China); Liu, Wenpeng; Zhang, Qingli; Peng, Fang; Luo, Jianqiao; Sun, Guihua; Sun, Dunlu [Chinese Academy of Sciences, Anhui Institute of Optics and Fine Mechanics, Hefei, Anhui Province (China)

2017-01-15

A mixed laser crystal of Nd-doped GYNO crystal was grown successfully by Czochralski method. The crystal belongs to monoclinic system with space group I2/a, the structural parameters are obtained by the X-ray Rietveld refinement method. The defects and dislocations along three crystallographic orientations were studied by using the chemical etching method with the phosphoric acid etchant. The mechanical properties (including hardness, yield strength, fracture toughness, and brittle index) of the crystal were estimated by Vickers hardness test. The transmission spectrum was measured at room temperature, and the absorption peaks were assigned. Spectral properties of the as-grown crystal were investigated by Judd-Ofelt theory, and the Judd-Ofelt intense parameters Ω{sub 2,4,6} were obtained to be 9.674 x 10{sup -20}, 2.092 x 10{sup -20}, and 4.061 x 10{sup -20} cm{sup 2}, respectively. (orig.)

Optical properties of CaWO4 and CaMoO4 crystals in the 4-25 eV region

International Nuclear Information System (INIS)

Grasser, R.; Pitt, E.; Scharmann, A.; Zimmerer, G.

1975-04-01

The reflection spectra of CaWO 4 and CaMoO 4 single crystals were measured in the region between 4 and 25 eV. The measurements were performed using the electron synchrotron DESY as a light source. Both crystals show very similar spectral features. A relatively sharp, well separated low energy peak is accompanied on the high energy side by two groups of maxima, each group containing three broad main reflection bands which strongly overlap. Besides this, a less pronounced structure is observed over the whole spectral region. The experimental results are discussed in terms of semiempirical MO calculations of the anionic transition metal oxo complexes. (orig.) [de

Electron paramagnetic resonance and optical absorption study of V{sup 4+} centres in YVO{sub 4} crystals

Energy Technology Data Exchange (ETDEWEB)

Garces, N Y [Department of Physics, West Virginia University, Morgantown, WV 26506 (United States); Stevens, K T [Northrop Grumman Space Technology, Synoptics, Charlotte, NC 28273 (United States); Foundos, G K [Northrop Grumman Space Technology, Synoptics, Charlotte, NC 28273 (United States); Halliburton, L E [Department of Physics, West Virginia University, Morgantown, WV 26506 (United States)

2004-10-06

Electron paramagnetic resonance (EPR) has been used to characterize three distinct V{sup 4+} centres in undoped Czochralski-grown yttrium orthovanadate (YVO{sub 4}) crystals. These EPR signals are observed at low temperatures, and their average c-axis splittings between adjacent {sup 51}V hyperfine lines are 40 G, 123 G, and 140 G. We refer to these centres as [V{sup 4+}]{sub A}, [V{sup 4+}]{sub B}, and [V{sup 4+}]{sub C}, respectively. The [V{sup 4+}]{sub A} and [V{sup 4+}]{sub B} centres are present in as-grown crystals. Exposure at 77 K to ionizing radiation (x-rays or an ultraviolet laser beam) destroys these centres and creates the [V{sup 4+}]{sub C} centres. The as-grown state of the crystal is restored upon returning to room temperature. Angular dependence data are used to determine the principal values and principal directions of the g tensor and the {sup 51}V hyperfine tensor for each of the centres. We suggest that the [V{sup 4+}]{sub A} centre is a V{sup 4+} ion adjacent to an oxygen vacancy and that the [V{sup 4+}]{sub B} centre is a V{sup 4+} ion substituting for a Y{sup 3+} ion (i.e. a vanadium antisite defect). The [V{sup 4+}]{sub C} centre is assigned to a V{sup 4+} ion at a regular vanadium site with a nearby stabilizing defect, possibly a Zr{sup 4+} on a Y{sup 3+} site. In as-grown crystals, there is a correlation between the number of [V{sup 4+}]{sub A} centres and the intensity (at 380 nm) of a broad near-edge optical absorption band. This band, now associated with oxygen vacancies, gives YVO{sub 4} a 'yellow' appearance.

Growth of methyl 2-(2,4-dinitrophenyl)aminopropanoate single crystals

Science.gov (United States)

Perigaud, A.; Nicolau, Y. F.

1986-12-01

Methyl 2-(2,4-dinitrophenyl)aminopropanoate single crystals, 1 cm in diameter and 7 cm in length have been grown by a travelling-heater-Bridgman method in polyethylene tubes introduced into glass ampoules, at a growth rate of 1.5-6 mm/day. The starting material was synthesised and purified by recrystallization from methanol and by vacuum evaporation to a purity of 99.994%. The period of growth, and hence the length of the crystal, is limited due to melt decomposition and polycondensation. The b-axis of the crystals is always oriented at about 72° to the ampoule axis. Good quality single crystals have been obtained giving a FWHM of the Cu Kα (040) rocking curve of about 1'.

Crystal growth and structure of KLnP/sub 4/O/sub 12/

International Nuclear Information System (INIS)

Guangyan, H.; Shuzhen, L.; Shuying, Y.; Mingyu, C.

1985-01-01

Potassium rare earth tetraphosphates KLnP/sub 4/O/sub 12/ are a kind of polyphosphates of rare earths with unique properties and structures. KNdP/sub 4/O/sub 12/ is a high-Nd-concentration laser material with a non-centrosymmetric space group P2, yielding linear and nonlinear optical properties. α-KErP/sub 4/O/sub 12/ might be used as a material for engineering device purpose. KTbP/sub 4/O/sub 12/ can emit strong green fluorescence, it might be a kind of a new crystal material for laser or luminescence. In order to search for new crystal materials and to study the correlations among the composition, structures and the properties of rare earth compounds, the crystal growth of KLnP/sub 4/O/sub 12/ and their structures are studied in this paper

Crystal structure of the human 4-1BB/4-1BBL complex.

Science.gov (United States)

Gilbreth, Ryan N; Oganesyan, Vaheh Y; Amdouni, Hamza; Novarra, Shabazz; Grinberg, Luba; Barnes, Arnita; Baca, Manuel

2018-05-02

4-1BBL is a member of the TNF superfamily and is the ligand for the TNFRsuperfamily receptor, 4-1BB. 4-1BB plays an immunomodulatory role in T cells and NK cells and agonists of this receptor have garnered strong attention as potentialimmunotherapy agents. Broadly speaking, the structural features of TNF superfamilymembers, their receptors and ligand/receptor complexes are similar. However, apublished crystal structure of human 4-1BBL suggests that it may be unique in thisregard, exhibiting a three-bladed propeller-like trimer assembly that is distinctly different from that observed in other family members. This unusual structure also suggests that the human 4-1BB/4-1BBL complex may be structurally unique within the TNF/TNFR superfamily, but to date no structural data have been reported. Here we report the crystal structure of the human 4-1BB/4-1BBL complex at 2.4 Å resolution. In this structure, 4-1BBL does not adopt the unusual trimer assembly previously reported, but instead forms a canonical bell-shaped trimer typical of other TNF superfamily members. The structure of 4-1BB is also largely canonical as is the 4-1BB/4-1BBL complex. Mutational data support the 4-1BBL structure reported here as being biologically relevant, suggesting that the previously reported structure is not. Together, the data presented here offer insight into structure/function relationships in the 4-1BB/4-1BBL system and improve our structural understanding of the TNF/TNFR superfamily more broadly. Published under license by The American Society for Biochemistry and Molecular Biology, Inc.

Crystallization and Characterization of a New Magnesium Sulfate Hydrate MgSO4.11H2O

NARCIS (Netherlands)

Genceli, F.E.; Lutz, M.; Spek, A.L.; Witkamp, G.J.

2007-01-01

The MgSO4 crystal hydrate formed below approximately 0 °C was proven to be the undecahydrate, MgSO4 • 11H2O (meridianiite) instead of the reported dodecahydrate MgSO4 • 12H2O. The crystals were grown from solution by eutectic freeze and by cooling crystallization. The crystal structure analysis and

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

Science.gov (United States)

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.

Crystal structure and characterization of the novel NH+⋯N hydrogen bonded polar crystal [NH2(CH2)4NH][BF4

Science.gov (United States)

Wojtaś, M.; Gaģor, A.; Czupiński, O.; Medycki, W.; Jakubas, R.

2012-03-01

Dielectric properties and phase transitions of the piperazinium tetrafluoroborate ([NH2(CH2)4NH][BF4], abbreviated as PFB) crystal are related to the one-dimensional arrangement of the cations linked by the bistable NH+⋯N hydrogen bonds and molecular motions of the [BF4]- units. The crystal structure of [NH2(CH2)4NH][BF4] is monoclinic at room temperature with the polar space group Pn. The polar/acentric properties of the room temperature phase IV have been confirmed by the piezoelectric and pyroelectric measurements. DSC measurements show that the compound undergoes three first-order structural phase transitions: at 421/411 K (heating/cooling), at 386/372 K and at 364/349 K. 1H and 19F NMR measurements indicate the reorientational motions of [BF4]- anions and piperazinium(+) cations as well as the proton motion in the hydrogen-bonded chains of piperazine along the [001] direction. Over the phase I the isotropic reorientational motions or even self-diffusion of the cations and anions are expected. The conductivity measurements in the vicinity of the II-I PT indicate a superionic phase over the phase I.

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

Science.gov (United States)

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.

Crystal structure of ethyl 2-(diethoxyphosphoryl-2-(2,3,4-trimethoxyphenylacetate

Directory of Open Access Journals (Sweden)

Moritz Schubert

2014-09-01

Full Text Available The title compound, C17H27O8P, was prepared by Michaelis–Arbuzov reaction of ethyl 2-bromo-2-(2,3,4-trimethoxyphenylacetate and triethyl phosphite. Such compounds rarely crystallize, but single crystals were recovered after the initial oil was left for approximately 10 years. The bond angle of the sp3-hybridized C atom connecting the benzene derivative with the phospho unit is widened marginally [112.5 (2°]. The terminal P—O bond length of 1.464 (2 Å clearly indicates a double bond, whereas the two O atoms of the ethoxy groups connected to the phosphorous atom have bond lengths of 1.580 (2 Å and 1.581 (3 Å. The three methoxy groups emerge out of the benzene-ring plane due to steric hindrance [C—C—O—C torsion angles = −179.9 (3°, −52.9 (4° and 115.3 (4°]. In the crystal, inversion dimers linked by pairs of C—H...O=P hydrogen bonds generate R22(14 loops. The chosen crystal was modelled as a non-merohedral twin.

Elastic properties of Cs2HgBr4 and Cs2CdBr4 crystals

International Nuclear Information System (INIS)

Kityk, A.V.; Zadorozhna, A.V.; Shchur, Y.I.; Martynyuk-Lototska, Y.I.; Burak, Y.; Vlokh, O.G.

1998-01-01

Using ultrasonic velocity measurements, all components of the elastic constant matrix C ij , elastic compliances matrix S ij , and linear compressibility constants matrix K ij of orthorhombic Cs 2 HgBr 4 and Cs 2 CdBr 4 crystals have been determined over a wide temperature range, including the region of the phase transition from the normal to the incommensurate phase. Results obtained are considered within the framework of the phenomenological theory. Preliminary analysis of the acoustical properties at room temperature clearly indicates that both crystals are relatively important materials for acousto-optical applications. Copyright (1998) CSIRO Australia

Yb3+:Sr3Y2(BO3)4: A potential ultrashort pulse laser crystal

International Nuclear Information System (INIS)

Sun, Shijia; Xu, Jinlong; Wei, Qi; Lou, Fei; Huang, Yisheng; Yuan, Feifei; Zhang, Lizhen; Lin, Zhoubin; He, Jingliang; Wang, Guofu

2015-01-01

Highlights: • A Yb 3+ :Sr 3 Y 2 (BO 3 ) 4 crystal was grown successfully by Czochralski method. • The crystal has wide absorption and emission bandwidth. • 3.47 W continuous wave laser output with a slope efficiency of 29% was obtained. • The results show that the crystal is a promising ultrashort pulse laser material. - Abstract: A Yb 3+ :Sr 3 Y 2 (BO 3 ) 4 crystal was grown successfully by the Czochralski method. The polarized spectral properties and continuous wave laser output of this crystal were investigated in detail. The crystal has larger absorption and emission cross sections compared with many mature Yb 3+ -doped borate crystals. The full width at half maximum of the emission bands around 1023 nm are 69 nm (E//a), 61 nm (E//b) and 65 nm (E//c). 3.47 W continuous wave laser output with a slope efficiency of 29% and an optical conversion efficiency of 24% was obtained. The results reveal that Yb 3+ :Sr 3 Y 2 (BO 3 ) 4 crystal is an excellent candidate for ultrashort pulse laser crystal

Gallium hole traps in irradiated KTiOPO{sub 4}:Ga crystals

Energy Technology Data Exchange (ETDEWEB)

Grachev, V.; Meyer, M.; Malovichko, G. [Physics Department, Montana State University, Bozeman, Montana 59717 (United States); Hunt, A. W. [Idaho Accelerator Center, Idaho State University, Pocatello, Idaho 83209 (United States)

2014-12-07

Nominally pure and gallium doped single crystals of potassium titanyl phosphate (KTiOPO{sub 4}) have been studied by Electron Paramagnetic Resonance at low temperatures before and after irradiation. Irradiation with 20 MeV electrons performed at room temperature and liquid nitrogen temperature caused an appearance of electrons and holes. Gallium impurities act as hole traps in KTiOPO{sub 4} creating Ga{sup 4+} centers. Two different Ga{sup 4+} centers were observed, Ga1 and Ga2. The Ga1 centers are dominant in Ga-doped samples. For the Ga1 center, a superhyperfine structure with one nucleus with nuclear spin ½ was registered and attributed to the interaction of gallium electrons with a phosphorus nucleus or proton in its surrounding. In both Ga1 and Ga2 centers, Ga{sup 4+} ions substitute for Ti{sup 4+} ions, but with a preference to one of two electrically distinct crystallographic positions (site selective substitution). The Ga doping eliminates one of the shortcomings of KTP crystals—ionic conductivity of bulk crystals. However, this does not improve significantly the resistance of the crystals to electron and γ-radiation.

Growth, crystal structure, spectral properties and laser performance of Yb3+:NaLu(MoO4)2 crystal

International Nuclear Information System (INIS)

Yu, Yi; Zhang, Lizhen; Huang, Yisheng; Lin, Zhoubin; Wang, Guofu

2013-01-01

A double molybdate Yb 3+ :NaLu(MoO 4 ) 2 crystal was successfully grown from a flux of Na 2 Mo 2 O 7 by the top-seeded solution growth method, for the first time to our knowledge. The crystal belongs to the tetragonal system with space group I4 1 /a, and the unit-cell parameters are a = b = 5.159 Å, c = 11.246 Å. Na and Lu atoms co-occupy the same lattice site, which leads to the disordered structure of NaLu(MoO 4 ) 2 crystal. The thermal expansion coefficients of the crystal are 1.35 × 10 −5 K −1 along the c-axis, and 1.01 × 10 −5 K −1 along the a-axis. The full-width at half-maximum of the emission bands are 67 nm for the σ-polarization and 50 nm for the π-polarization at about 1020 nm. The maximum emission cross-sections for the σ- and π-polarizations are 2.79 × 10 −20 cm 2 and 2.94 × 10 −20 cm 2 , respectively. 0.3 W output power at 1025 nm was obtained at an absorbed pump power of 1.7 W, with a slope efficiency of 24%. (paper)

Crystal structure of 2-[4(E-2,6-bis(4-chlorophenyl-3-ethylpiperidin-4-ylidene]acetamide

Directory of Open Access Journals (Sweden)

K. Priya

2015-11-01

Full Text Available In the title piperidine derivative, C21H22Cl2N2O, the piperidine ring adopts a chair conformation. The chlorophenyl rings are oriented at an angle of 45.59 (14° with respect to each other. In the crystal, molecules are linked via N—H...O hydrogen bonds, forming C(4 chains along [100]. The chains are linked by C—H...O hydrogen bonds, forming sheets parallel to the ab plane. Within the sheets, there are N—H...π interactions present. The crystal studied was refined as an inversion twin.

Crystal structures of the all-cysteinyl-coordinated D14C variant of Pyrococcus furiosus ferredoxin: [4Fe–4S] ↔ [3Fe–4S] cluster conversion

DEFF Research Database (Denmark)

Løvgreen, Monika Nøhr; Martic, Maja; Windahl, Michael S.

2011-01-01

The structure of the all-cysteinyl-coordinated D14C variant of [4Fe–4S] ferredoxin from the hyperthermophilic archaeon Pyrococcus furiosus has been determined to 1.7 Å resolution from a crystal belonging to space group C2221 with two types of molecules, A and B, in the asymmetric unit. A and B...... molecules have different crystal packing and intramolecular disulfide bond conformation. The crystal packing reveals a β-sheet interaction between A molecules in adjacent asymmetric units, whereas B molecules are packed as monomers in a less rigid position next to the A–A extended β-sheet dimers...... and purification are carried out at pH 5.8, only the monomer is obtained. The crystal structure of D14C [3Fe–4S] P. furiosus ferredoxin monomer was determined to 2.8 Å resolution from a crystal belonging to space group P212121 with two molecules in the asymmetric unit. The molecules resemble molecule A of D14C [4...

Crystal field parameters in UCl4: Experiment versus theory

International Nuclear Information System (INIS)

Zolnierek, Z.; Gajek, Z.; Khan Malek, C.

1984-01-01

Crystal field effect on U 4+ ion with the 3 H 4 ground term in tetragonal ligand field of UCl 4 has been studied in detail. Crystal field parameters determined experimentally from optical spectroscopy and magnetic susceptibility are in good agreement with CEP sets derived from the modified point charge model and the ab initio method. Theoretical calculations lead to overestimating the A 4 4 4 > and lowering the A 2 0 2 > values in comparison to those found in the experiments. The discrepancies are, however, within an accuracy of calculations. A large reduction of expectation values of the magnetic moment operator for the eigenvectors of lowest CF levels (17.8%), determined from magnetic susceptibility, cannot be attributed to the overlap and covalency effects only. The detailed calculations have shown that the latter effects provide about 4.6% reduction of respective matrix elements, and the applied J-J mixing procedure increases this factor up to 6.5%. Since similar, as in UCl 4 , reduction factor (proportional15%) has already been observed in a number of different uranium compounds, it seems to be likely that this feature is involved in the intrinsic properties of the U 4+ ion. We endeavor to explain this effect in terms of configuration interaction mechanisms. (orig.)

Comparative study of optical and scintillation properties of YVO4, (Lu0.5Y0.5)VO4, and LuVO4 single crystals

International Nuclear Information System (INIS)

Fujimoto, Yutaka; Yanagida, Takayuki; Yokota, Yuui; Chani, Valery; Kochurikhin, Vladimir V.; Yoshikawa, Akira

2011-01-01

Optical and scintillation properties of YVO 4 , (Lu 0.5 Y 0.5 )VO 4 , and LuVO 4 single crystals grown by the Czochralski (CZ) method with RF heating system are compared. All vanadate crystals show high transmittance (∼80%) in the 400-900 nm wavelength range. In both photo- and radio-luminescence spectra, intense peak around 400-500 nm, which was ascribed to the transition from triplet state of VO 4 3- , was clearly observed. The main decay time component was about 38 μs (YVO 4 ), 18 μs ((Lu 0.5 Y 0.5 )VO 4 ), and 17 μs (LuVO 4 ) under 340 nm excitation. The scintillation light yields of YVO 4 , (Lu 0.5 Y 0.5 )VO 4 , and LuVO 4 crystals (obtained from the 137 Cs excited pulse height spectra) were evaluated to be about 11,200, 10,700, and 10,300 ph/MeV, respectively.

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

Science.gov (United States)

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.

Crystallization of [Fe4S3]-ferredoxin from the hyperthermophile archaeon pyrococcus furiosus

DEFF Research Database (Denmark)

Nielsen, Michael Ericsson Skovbo; Harris, Pernille; Christensen, Hans Erik Mølager

2003-01-01

Recombinant Pyrococcus furiosus ferredoxin with a [Fe3S4]-cluster was crystallized through steps of optimization and X-ray diffraction data were collected from several crystal forms. Flat plate-like crystals were grown by hanging-drop vapour diffusion. The precipitant used was 30% PEG 400; the p...

Photoacoustic and dielectric spectroscopic studies of 4-dimethylamino-n-methyl-4-stilbazolium tosylate single crystal: An efficient terahertz emitter

Science.gov (United States)

Manivannan, M.; Martin Britto Dhas, S. A.; Jose, M.

2016-12-01

Bulk terahertz emitting single crystal of 4-dimethylamino-N-methyl-4-stilbazolium tosylate (DAST) was synthesized by condensation method and grown by slow solvent evaporation technique from methanol. The structure and cell parameters of the grown crystals were derived from single crystal and powder X-ray diffraction analyses and the optical properties of the crystal were analyzed by UV-Vis Spectrophotometer. The presence of functional groups was identified by FTIR and FT-Raman spectroscopic studies. We demonstrated that in DAST crystal, the thermal transport properties such as thermal conductivity, thermal diffusivity and thermal effusivity are better than several well recognized standard materials using photoacoustic spectrophotometer. The dielectric measurement was made as a function of frequency (1 Hz-35 MHz) at different temperatures (30-200 °C). The dielectric constant and dielectric loss were found to be strongly dependent on temperature and frequency of the applied electric field. The semicircle in the cole-cole plot showed the presence of dielectric relaxation in the crystal with its diameter representing the resistance of the crystal. The resistivity and ac conductivity were calculated from the measured dielectric data.

Spectral properties and laser performance of Tm, Ho: LuLF4 crystal

Science.gov (United States)

Peng, Haiyan; Zhang, Kun; Zhang, Lianhan; Hang, Yin; Xu, Jianqiu; Tang, Yulong; Cheng, Yan; Xiong, Jing

2008-12-01

LuLiF4 single crystals co-doped with thulium (5%) and holmium (0.5%), which had large size, intact shape and high optical quality, were successfully grown by the medium frequency induction heating Czochralski Technique. The absorption spectrum of the crystals showed that the main absorption peak located at 686 nm and 792nm. At room temperature, LuLiF4 single crystals co-doped with thulium (5%) and holmium (0.5%) were end-pumped by a fiber-coupled laser diode system with pumping wavelength of 795 nm. We achieved power of 50 mw continuous laser output at 2.05 μm wavelength.

Thermal characterization, crystal field analysis and in-band pumped laser performance of Er doped NaY(WO(4(2 disordered laser crystals.

Directory of Open Access Journals (Sweden)

María Dolores Serrano

Full Text Available Undoped and Er-doped NaY(WO42 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 Er(3+ levels up to (4G(7/2 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 (4I(13/2↔(4I(15/2 laser related transition have been determined at 77 K. The (4I(13/2 Er(3+ 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 (4I(13/2 multiplet at λ≈1500 nm with a broadband (FWHM≈20 nm diode laser source perfectly matching the 77 K crystal (4I(15/2 → (4I(13/2 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.

Crystal structure of 4-aminobenzoic acid–4-methylpyridine (1/1

Directory of Open Access Journals (Sweden)

M. Krishna Kumar

2015-02-01

Full Text Available In the title 1:1 adduct, C6H7N·C7H7NO2, the carboxylic acid group is twisted at an angle of 4.32 (18° with respect to the attached benzene ring. In the crystal, the carboxylic acid group is linked to the pyridine ring by an O—H...N hydrogen bond, forming a dimer. The dimers are linked by N—H...O hydrogen bonds, generating (010 sheets.

Crystal structure of ethyl (4R-2-amino-7-hydroxy-4-phenyl-4H-chromene-3-carboxylate

Directory of Open Access Journals (Sweden)

Joel T. Mague

2015-07-01

Full Text Available In the title compound, C18H17NO4, the dihedral angle between the phenyl ring and the fused six-membered ring is 77.65 (4°. The conformation of the molecule is determined in part by an intramolecular N—H...O hydrogen bond between the amino H atom and the carbonyl O atom, forming an S(6 motif. In the crystal, molecules are linked into N—H...O hydrogen-bonded inversion dimers which are then connected into chains along [001], forming a two-dimensional network parallel to (100 via O—H...O hydrogen bonds. C—H...O interactions further contribute to the crystal stability. The ethyl group is disordered over two sets of sites in a 0.801 (5:0.199 (5 ratio.

Laser-induced damage investigation at 1064 nmin KTiOPO4 crystals and its analogy with RbTiOPO4

International Nuclear Information System (INIS)

Hildenbrand, A.; Wagner, F. R.; Akhouayri, H.; Natoli, J.-Y.; Commandre, M.; Theodore, F.; Albrecht, H.

2009-01-01

Bulk laser-induced damage at 1064 nm has been investigated in KTiOPO4 (KTP) and RbTiOPO4 (RTP) crystals with a nanosecond pulsed Nd:YAG laser. Both crystals belong to the same family. Throughout this study, their comparison shows a very similar laser-damage behavior. The evolution of the damage resistance under a high number of shots per site (10,000 shots) reveals a fatigue effect of KTP and RTP crystals. In addition, S-on-1 damage probability curves have been measured in both crystals for all combinations of polarization and propagation direction aligned with the principal axes of the crystals. The results show an influence of the polarization on the laser-induced damage threshold (LIDT), with a significantly higher threshold along the z axis, whereas no effect of the propagation direction has been observed. This LIDT anisotropy is discussed with regard to the crystallographic structure.

Characterization of mixed Nd :LuxGd1-xVO4 laser crystals

Science.gov (United States)

Yu, H. H.; Zhang, H. J.; Wang, Z. P.; Wang, J. Y.; Yu, Y. G.; Cheng, X. F.; Shao, Z. S.; Jiang, M. H.; Ling, Z. C.; Xia, H. R.

2007-06-01

A series of laser crystals Nd :LuxGd1-xVO4 (x=0.14,0.32,0.50,0.61,0.70,0.80) was grown by the Czochralski method. The thermal properties, including the average linear thermal expansion coefficients, thermal diffusion coefficients, specific heats, and thermal conductivities, of the mixed crystals were obtained. The material constants Ms for the thermal stress resistance figure were calculated and showed that the thermal fracture limits of the mixed crystals should be comparable with that of Nd :YVO4. The polarization absorption spectra from 240to1000nm were measured at room temperature and the absorption cross sections at 809nm were calculated. Using the Judd-Ofelt theory, the theoretical radiative lifetimes were calculated and compared with the experimental results. Continuous wave laser performances were achieved with the mixed crystals at the wavelength of 1.06μm when they were pumped by a laser diode. Thermal, optical, and laser properties have shown variation as a function of x and proved that the mixed crystals are good laser materials.

Morphologies of CaMoO sub 4 crystals in simulated nuclear waste disposal glass

Energy Technology Data Exchange (ETDEWEB)

Li, D.; Sengers, E.G.F.; Janssen, F.J.J.G. (KEMA, Arnhem (Netherlands). Chemical Technology and Material Research Dept.); Waal, H. de (TPO-TNO Glass Technology, Eindhoven (Netherlands))

1992-07-01

Fission products can diffuse through nuclear waste disposal glass due to the action of the temperature gradient caused by radioactive decay and the small thermal conductivity of the glass. Diffusion may eventually lead to crystallization. Because the densities of the products of glass crystallization may differ from that of the parent glass, crystallization causes stresses to develop, which can lead to fracture and exposure of increased surface area to environmental attack. Several kinds of crystals including, CaMoO{sub 4}, in the simulated nuclear waste disposal glass K{sub 3}, which consists of Na{sub 2}O, B{sub 2}O{sub 3}, SiO{sub 2} and other oxides, were identified previously after heat treatment. Recently it was found that CaMoO{sub 4} crystals have two kinds of morphologies in glass K{sub 3} heat-treated at temperatures between 870 and 1120 K. One kind of morphology, which is rather special, has not previously been reported. In this letter the morphologies of CaMoO{sub 4} crystals in this simulated nuclear waste disposal glass are discussed. (author).

Growth of 4-(dimethylamino) benzaldehyde doped triglycine sulphate single crystals and its characterization

International Nuclear Information System (INIS)

Rai, Chitharanjan; Sreenivas, K.; Dharmaprakash, S.M.

2009-01-01

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 deg. C/min. An increase in the Curie temperature T c =51 deg. C (for pure TGS, T c =48.5 deg. 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.

Growth of 4-(dimethylamino) benzaldehyde doped triglycine sulphate single crystals and its characterization

Science.gov (United States)

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.

Refractometry of LiRbSO4 crystals

International Nuclear Information System (INIS)

Stadnyk, V.Y.; Romanyuk, M.O.; Karplyuk, L.T.

2004-01-01

Making use of the Obreimov photographic method, the dependences of birefringence Δn i of LiRbSO 4 crystals have been studied in wide spectral (250-800 nm) and temperature (100 - 600 K) ranges, as well as the influence of uniaxial mechanical stresses on them. The anomalies of Δn i at successive phase transitions, namely, paraelectric - incommensurate - commensurate ferroelastic - ferroelectric - paraelectric phases, have been discovered

Crystal structure of 2-isopropyl-4-methoxy-5-methylphenyl 4-methylbenzenesulfonate

Directory of Open Access Journals (Sweden)

Yassine Laamari

2018-03-01

Full Text Available The title compound, C18H22O4S, an hemisynthetic product, was obtained by the tosylation reaction of the naturally occurring meroterpene p-methoxythymol. The molecule comprises a tetrasubstitued phenyl ring linked to a toluenesulfonate through one of its O atoms. In the crystal, C—H...O and C—H...π interactions link the molecules, forming a three-dimensional network.

Bulk crystal growth and their effective third order nonlinear optical properties of 2-(4-fluorobenzylidene) malononitrile (FBM) single crystal

Science.gov (United States)

Priyadharshini, A.; Kalainathan, S.

2018-04-01

2-(4-fluorobenzylidene) malononitrile (FBM), an organic third order nonlinear (TONLO) single crystal with the dimensions of 32 × 7 × 11 mm3, has been successfully grown in acetone solution by slow evaporation technique at 35 °C. The crystal system (triclinic), space group (P-1) and crystalline purity of the titular crystal were measured by single crystal and powder X-ray diffraction, respectively. The molecular weight and the multiple functional groups of the FBM material were confirmed through the mass and FT-IR spectral analysis. UV-Vis-NIR spectral study enroles that the FBM crystal exhibits excellent transparency (83%) in the entire visible and near infra-red region with a wide bandgap 2.90 eV. The low dielectric constant (εr) value of FBM crystal is appreciable for microelectronics industry applications. Thermal stability and melting point (130.09 °C) were ascertained by TGA-DSC analysis. The laser-induced surface damage threshold (LDT) value of FBM specimen is found to be 2.14 GW/cm2, it is fairly good compared to other reported NLO crystals. The third - order nonlinear optical character of the FBM crystal was confirmed through the typical single beam Z-scan technique. All these finding authorized that the organic crystal of FBM is favorably suitable for NLO applications.

Optical diagnostics of lead and PbGa2S4 layered crystal laser plasmas

International Nuclear Information System (INIS)

Shuaibov, A.K.; Dashchenko, A.I.; Shevera, I.V.

2001-01-01

Paper presents the results of the optic diagnostics of plasma of laser flames formed from lead surface and PbGa 2 S 4 laminar crystal using a neodymium laser. It is shown that the most intensive lines in the lead laser plasma are as follows: 405.7, 368.3, 364.0 nm PbI and 220.4 nm PbII while for the laminar crystal base plasma - the combination of the most intensive lines of PbI and GaI emission. One determined the narrow point of recombination fluxes for the ion and the atomic components of laser plasma of lead and of PbGa 2 S 4 crystal. One conducted comparison study of emission dynamics of PbI and GaI lines in laser plasma of the respective metals and of PbGa 2 S 4 crystal [ru

Polarized spectroscopic properties of Nd3+-doped KGd(WO4)2 single crystal

International Nuclear Information System (INIS)

Chen Yujin; Lin Yanfu; Gong Xinghong; Tan Qiguang; Zhuang Jian; Luo Zundu; Huang Yidong

2007-01-01

The polarized absorption spectra, infrared fluorescence spectra, upconversion visible fluorescence spectra, and fluorescence decay curve of orientated Nd 3+ :KGd(WO 4 ) 2 crystal were measured at room-temperature. Some important spectroscopic parameters were investigated in detail in the framework of the Judd-Ofelt theory and the Fuchtbauer-Ladenburg formula. The effect of the crystal structure on the spectroscopic properties of the Nd 3+ ions was analyzed. The relation among the spectroscopic parameters and the laser performances of the Nd 3+ :KGd(WO 4 ) 2 crystal was discussed

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

International Nuclear Information System (INIS)

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

2012-01-01

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. - Graphical abstarct: Exploiting phase diagram study and solvent free synthesis a novel compound was synthesized and its single crystal growth, atomic packing, energy band gap and refractive index were studied. Highlights: ► Novel organic complex was synthesized using Green or solvent free synthesis. ► Phase diagram study provided the information to identify the worthy composition of novel complex. ► The single crystal of the sufficient size was grown from the ethanol solution. ► Crystal analysis suggested that the covalent bond is formed between the two parent compounds. ► The transmittance of the crystal was found to be 70% and it was transparent from 412 to 850 nm.

The crystal structure of the phosphatidylinositol 4-kinase IIalpha

Czech Academy of Sciences Publication Activity Database

Bäumlová, Adriana; Chalupská, Dominika; Rozycki, B.; Jovic, M.; Wisniewski, E.; Klíma, Martin; Dubánková, Anna; Kloer, D. P.; Nencka, Radim; Balla, T.; Bouřa, Evžen

2015-01-01

Roč. 22, č. 1 (2015), s. 5 ISSN 1211-5894. [Discussions in Structural Molecular Biology. Annual Meeting of the Czech Society for Structural Biology /13./. 19.03.2015-21.03.2015, Nové Hrady] EU Projects: European Commission(XE) 333916 - STARPI4K Institutional support: RVO:61388963 Keywords : PI4K IIalpha * crystal structure Subject RIV: CE - Biochemistry

Studies on synthesis, structural, luminescent and thermal properties of a new non-linear optical crystal: 4-amino-4H-1,2,4-triazol-1-ium-3-hydroxy-2,4,6-trinitrophenolate

Energy Technology Data Exchange (ETDEWEB)

Dhamodharan, P.; Sathya, K.; Dhandapani, M., E-mail: chemistrydhandapani@gmail.com

2017-03-01

A new organic proton transfer complex having NLO activity, 4-amino-4H-1,2,4-triazol-1-ium-3-hydroxy-2,4,6-trinitrophenolate (ATHTP), was crystallized to investigate the factors which stabilize the structure of the crystal. The compound crystallizes in triclinic system with space group P-1. Elemental analysis, thermal analysis, UV–Vis–NIR, FT-IR and NMR spectral analyses were carried out to characterize the crystal. Optical, spectral and thermal properties of the title crystal were analyzed to recommend the material for optical applications. Z-scan was used to measure the effective third-order nonlinear optical susceptibility and nonlinear refractive index. The crystal structure was determined using single crystal XRD method and the structure was optimized using Gaussian 09 program at B3LYP/6-311++G(d,p) level of basis set. This hydrogen bond interactions led to the increase in first-order hyperpolarizability of ATHTP and was 30 times greater than that of urea. Hirshfeld analyses surface analysis was carried out to explore intermolecular interactions in the crystalline state. - Highlights: • Single crystals were grown by slow evaporation solution growth technique. • N-H…O, O-H…O and C-H…O type of interactions lead to stable network. • The thermal stability of the compound was investigated by TG/DTA analyses. • The third-order nonlinear optical susceptibility is found to be 2.1×10{sup −7} esu. • Hirshfeld analyses explore covalent and non covalent interactions.

Redox process catalysed by growing crystal-strengite, FePO4,2H2O, crystallizing from solution with iron(II) and hydroxylamine

Science.gov (United States)

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.

The determination, by X-ray-fluorescence spectrometry, of tin and tungsten in ores, concentrates, and residues of scheelite, wolframite, and cassiterite

International Nuclear Information System (INIS)

Balaes, A.M.E.; Jacobs, J.J.; Bray, A.R.; Kendrick, K.

1983-01-01

The method of analysis described is applicable to samples with tin and tungsten contents from 15p.p.m. to 75 per cent. For samples containing tin and tungsten in the range 2000p.p.m. to 75 per cent, the matrix variations are compensated for by the use of briquettes containing coarse river sand, the internal standard, and potassium chloride, the last of which acts as a binder, diluet, and grinding aid. For the samples containing tin and tungsten in the range 15p.p.m. to 2000p.p.m., the potassium chloride is omitted. Zinc and antimony are used as the internal standard for tungsten and tin respectively. Calibration graphs for tin and tungsten are obtained by the use of standard reference materials for cassiterite and scheelite. The precision of the analysis for tin ranges from a relative standard deviation of 0,039 at 50p.p.m. to 0,005 at 75 per cent. The values for tungsten are relatively constant at between 0,015 and 0,008 at concentrations between 50p.p.m. and 50 per cent. The lower limits of detection for tungsten and tin by the high-concentration technique of analysis are 202 and 155p.p.m. respectively, and by the low-concentration technique the corresponding limits are 4 and 2p.p.m. The overall time required for the analysis of ten samples by these techniques is approximately 3 hours. The laboratory method is detailed in an appendix

The oxidation of ReCl_5 with oleum: synthesis and crystal structure of Re_2O_4Cl_4(SO_4)

International Nuclear Information System (INIS)

Betke, Ulf; Wickleder, Mathias S.

2012-01-01

The reaction of ReCl_5 and fuming sulfuric acid (25 % SO_3) in a sealed glass tube at 200 C led to red, needle shaped single crystals of Re_2O_4Cl_4(SO_4) (monoclinic, C2/c, a = 1501.8(2) pm, b = 1545.9(2) pm, c = 945.18(8) pm, β = 98.761(9) , Z = 8). In the crystal structure the [ReO_2] moieties are linked by [SO_4]"2"- tetrahedra to chains along the [101] direction. Each sulfate ion connects four rhenium atoms, additional two chloride ions complete the octahedral coordination sphere of each rhenium atom according to "1_∞[ReO_2_/_1Cl_2_/_1(SO_4)_2_/_4]. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Crystal structure of (3S*,4R*-4-fluoro-3-(4-methoxyphenyl-1-oxo-2-phenyl-1,2,3,4-tetrahydroisoquinoline-4-carboxylic acid

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Anna Lehmann

2017-06-01

Full Text Available The title compound, C23H18FNO4, crystallized as a racemate. It exhibits a cis conformation with respect to the F atom and the methine H atom. The piperidine ring has a screw-boat conformation. The methoxyphenyl ring and the phenyl ring are inclined to the mean plane of the isoquinoline ring system by 89.85 (4 and 46.62 (5°, respectively, and by 78.15 (5° to one another. In the crystal, molecules are linked by an O—H...O hydrogen bond forming chains propagating along the a-axis direction. The chains are linked by C—H...F hydrogen bonds, forming layers lying parallel to the ab plane.

Surface relief grating formation on a single crystal of 4-(dimethylamino)azobenzene

International Nuclear Information System (INIS)

Nakano, Hideyuki; Tanino, Takahiro; Shirota, Yasuhiko

2005-01-01

Surface relief grating (SRG) formation on an organic single crystal by irradiation with two coherent laser beams has been demonstrated by using 4-(dimethylamino)azobenzene (DAAB). It was found that the SRG formation was greatly depending upon both the coordination of the crystal and the polarization of the writing beams. The dependence of the polarization of writing beams on the SRG formation using the single crystal was found to be quite different from that reported for amorphous polymers and photochromic amorphous molecular materials, suggesting that the mechanism of the SRG formation on the organic crystal is somewhat different from that on amorphous materials

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

Science.gov (United States)

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.

Calcium Sulfoaluminate Sodalite (Ca 4 Al 6 O 12 SO 4 ) Crystal Structure Evaluation and Bulk Modulus Determination

KAUST Repository

Hargis, Craig W.

2013-12-12

The predominant phase of calcium sulfoaluminate cement, Ca 4(Al6O12)SO4, was investigated using high-pressure synchrotron X-ray diffraction from ambient pressure to 4.75 GPa. A critical review of the crystal structure of Ca4(Al 6O12)SO4 is presented. Rietveld refinements showed the orthorhombic crystal structure to best match the observed peak intensities and positions for pure Ca4(Al6O 12)SO4. The compressibility of Ca4(Al 6O12)SO4 was studied using cubic, orthorhombic, and tetragonal crystal structures due to the lack of consensus on the actual space group, and all three models provided similar results of 69(6) GPa. With its divalent cage ions, the bulk modulus of Ca4(Al6O 12)SO4 is higher than other sodalites with monovalent cage ions, such as Na8(AlSiO4)6Cl2 or Na8(AlSiO4)6(OH)2·H 2O. Likewise, comparing this study to previous ones shows the lattice compressibility of aluminate sodalites decreases with increasing size of the caged ions. Ca4(Al6O12)SO4 is more compressible than other cement clinker phases such as tricalcium aluminate and less compressible than hydrated cement phases such as ettringite and hemicarboaluminate. © 2013 The American Ceramic Society.

Strong crystal field effect in Np{sup 4+}:ThCl{sub 4} - optical absorption study

Energy Technology Data Exchange (ETDEWEB)

Gajek, Z. [Instytut Niskich Temperatur i Badan Strukturalnych, Polska Akademia Nauk, 50-950 Wroclaw 2, Skr. Poczt. 1410 (Poland); Krupa, J.C. [Laboratoire de Radiochimie, Institut de Physique Nucleaire, BP 1, 91406 Orsay Cedex (France)

1998-12-21

Results of optical absorption measurements in polarized light on tetravalent neptunium diluted in a ThCl{sub 4} single crystal are reported. The recorded spectra are complex, pointing to the presence of an Np{sup 3+} impurity. The electronic transitions assigned to the Np{sup 4+} ion are interpreted in terms of the usual model, following the actual understanding of the neptunium electronic structure and independent theoretical predictions. R.m.s. deviations of the order of 36 cm{sup -1} have been obtained for 42 levels fitted with 11 free parameters. The crystal field effect resulting from the fitting is considerably larger than that observed for the uranium ion in the same host. (author)

Synthesis, Crystal Structure, DFT Study and Antifungal Activity of 4-(5-((4-Bromobenzyl thio-4-Phenyl-4H-1,2,4-Triazol-3-ylpyridine

Directory of Open Access Journals (Sweden)

Jin-Xia Mu

2015-12-01

Full Text Available The title compound 4-(5-((4-bromobenzylthio-4-phenyl-4H-1,2,4-triazol-3-ylpyridine (C20H15BrN4S was synthesized, and its structure was confirmed by 1H NMR, MS and elemental analyses and single-crystal X-ray structure determination. It crystallizes in the triclinic space group P-1 with a = 7.717(3, b = 9.210(3, c = 13.370(5 Å, α = 80.347(13, β = 77.471(13, γ = 89.899(16°, V = 913.9(6 Å3, Z = 2 and R = 0.0260 for 3145 observed reflections with I > 2σ(I. A Density functional theory (DFT (B3LYP/6-31G calculation of the title molecule was carried out. The full geometry optimization was carried out using a 6-31G basis set, and the frontier orbital energy. Atomic net charges are discussed. Calculated bond lengths and bond angles were found to differ from experimental values, and the compound exhibits moderate antifungal activity.

Thermal gravimetric analysis of the CsCuCl3, Cs2CuCl4 and Cs2CuCl4x2H2O crystals

International Nuclear Information System (INIS)

Soboleva, L.V.; Vasil'eva, M.G.

1977-01-01

The thermal characteristics of crystals of Cs 2 CuCl 4 , Cs 2 CuCl 4 x2H 2 O, and CsCuCl 3 were investigated thermogravimetrically. The derivatogram of the Cs 2 CuCl 4 crystal is characterized by the presence of a single endothermal effect at 505 deg C. The derivatogram of the Cs 2 CuCl 4 x2H 2 O crystal contains three endothermal effects: at 40, 135, and 480 deg C. The derivatogram of the CsCuCl 3 crystal shows the presence of two endothermal effects at 142 and 455 deg C. The thermogravimetric data on Cs 2 CuCl 4 and CsCuCl 3 crystals reveal crystal decomposition on melting; hence, these crystals cannot be grown from melts

Electrical and thermoluminescence properties of γ-irradiated La2CuO4 crystals

Science.gov (United States)

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.

Crystal field parameters in UCI 4: Experiment versus theory

Science.gov (United States)

Zolnierek, Z.; Gajek, Z.; Malek, Ch. Khan

1984-08-01

Crystal field effect on U 4+ ion with the 3H 4 ground term in tetragonal ligand field of UCl 4 has been studied in detail. Crystal field parameters determined experimentally from optical spectroscopy and magnetic susceptibility are in good agreement with CFP sets derived from the modified point charge model and the ab initio method. Theoretical calculations lead to overestimating the A44 and lowering the A02 values in comparison to those found in the experiments. The discrepancies are, however, within an accuracy of calculations. A large reduction of expectation values of the magnetic moment operator for the eigenvectors of lowest CF levels (17.8%), determined from magnetic susceptibility, cannot be attributed to the overlap and covalency effects only. The detailed calculations have shown that the latter effects provide about 4.6% reduction of respective matrix elements, and the applied J-J mixing procedure increases this factor up to 6.5%. Since similar, as in UCl 4, reduction factor(≈15%) has already been observed in a number of different uranium compounds, it seems likely that this feature is involved in the intrinsic properties of the U 4+ ion. We endeavor to explain this effect in terms of configuration interaction mechanisms.

Structural and optical properties of new organic crystal 1-[4-(methylsulfanyl) phenyl]-3-(2,4,5-trimethoxyphenyl) prop-2-en-1-One for optical limiting applications

Science.gov (United States)

Raghavendra, S.; Anil Kumar, K. V.; Chandra Shekhara Shetty, T.; Dharmaprakash, S. M.

2014-09-01

A new organic crystal belonging to chalcone family 1-[4-(methylsulfanyl) phenyl]-3-(2,4,5-trimethoxyphenyl) prop-2-en-1-One (4MSTP) with molecular formula C19H20O4S has been synthesized by Claisen Schimidt condensation method. 4MSTP was crystallized by slow evaporation technique using methanol solution at ambient temperature. Crystals of 4MSTP were characterized by Fourier transform infrared (FTIR) spectroscopy, NMR spectroscopy, single crystal and powder X-ray diffraction (XRD) technique, thermal analysis and UV-Vis spectroscopy. Nonlinear optical properties of 4MSTP crystals were investigated using Nd:YAG laser at 532 nm wavelength. The presence of functional groups were confirmed by FTIR and the structural elucidation was done using proton and carbon NMR spectral analysis. The X-ray diffraction peaks are indexed by the least square fit method. From the single crystal XRD study it is found that 4MSTP crystallizes in monoclinic system with a centro symmetric space group P21/c. The unit cell parameters of the crystal are: a = 19.2413(6) Å, b = 8.9504(3) Å, c = 10.3608(4) Å, α = 90°, β = 104.45°(2) and γ = 90°. Linear optical studies were carried out using UV visible spectral technique. The studies revealed that the 4MSTP crystals can be exploited for the nonlinear optical applications. TGA-DSC experiments indicated that the melting point of the material is 165.91 °C and the crystals showed absence of phase transition before melting point. Calculated excited state absorption (σex) is greater than the ground state absorption (σg) and thus the condition for Reverse Saturable Absorption (RSA) is achieved in 4MSTP. The open aperture Z-Scan curve showed minimum transmittance at the focus and hence 4MSTP crystals have maximum nonlinear absorption. The variation of nonlinear transmission with input intensity of laser showed that 4MSTP crystals can be used as an optical limiter.

Growth of 4-(dimethylamino) benzaldehyde doped triglycine sulphate single crystals and its characterization

Energy Technology Data Exchange (ETDEWEB)

Rai, Chitharanjan, E-mail: raichitharanjan@gmail.co [Department of Physics, Mangalore University, Mangalagangotri 574 199 (India); Kalpataru First Grade Science College, Tiptur 572 202 (India); Sreenivas, K. [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India); Dharmaprakash, S.M., E-mail: smdharma@yahoo.co [Department of Physics, Mangalore University, Mangalagangotri 574 199 (India)

2009-11-15

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 deg. C/min. An increase in the Curie temperature T{sub c}=51 deg. C (for pure TGS, T{sub c}=48.5 deg. 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.

Spectroscopic analysis and laser performance of Tm3+ : NaGd(MoO4)2 crystal

International Nuclear Information System (INIS)

Guo Weijie; Chen Yujin; Lin Yanfu; Gong Xinghong; Luo Zundu; Huang Yidong

2008-01-01

Detailed polarized spectral properties of Tm 3+ : NaGd(MoO 4 ) 2 crystal have been investigated. The room temperature absorption and fluorescence spectra were recorded. The fluorescence decay mechanisms of the 1 G 4 and 3 H 4 multiplets in Tm 3+ : NaGd(MoO 4 ) 2 crystal were discussed. Room temperature quasi-cw 1.9 μm laser emission from the Ti : sapphire laser pumped Tm 3+ : NaGd(MoO 4 ) 2 crystal has been demonstrated. The maximum output power of 170 mW has been achieved with a slope efficiency of 25%

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

Energy Technology Data Exchange (ETDEWEB)

Sharma, K.P.; Reddi, R.S.B.; Bhattacharya, S. [Department of Chemistry, Centre of Advance Study, Banaras Hindu University, Varanasi-221005 (India); Rai, R.N., E-mail: rn_rai@yahoo.co.in [Department of Chemistry, Centre of Advance Study, Banaras Hindu University, Varanasi-221005 (India)

2012-06-15

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. - Graphical abstarct: Exploiting phase diagram study and solvent free synthesis a novel compound was synthesized and its single crystal growth, atomic packing, energy band gap and refractive index were studied. Highlights: Black-Right-Pointing-Pointer Novel organic complex was synthesized using Green or solvent free synthesis. Black-Right-Pointing-Pointer Phase diagram study provided the information to identify the worthy composition of novel complex. Black-Right-Pointing-Pointer The single crystal of the sufficient size was grown from the ethanol solution. Black-Right-Pointing-Pointer Crystal analysis suggested that the covalent bond is formed between the two parent compounds. Black-Right-Pointing-Pointer The transmittance of the crystal was found to be 70% and it was transparent from 412 to 850 nm.

Growth and optical property of ZnWO4: Er3+ crystal

International Nuclear Information System (INIS)

Yang Fugui; Tu Chaoyang; Li Jianfu; Jia Guohua; Wang Hongyan; Wei Yanping; You Zhenyu; Zhu Zhaojie; Wang Yan; Lu Xiuai

2007-01-01

Good quality crystals ZnWO 4 activated with Er 3+ have been grown by means of Czochralski method and characterized using optical spectroscopy techniques. XRD, absorption spectra, fluorescence spectrum are presented and the Judd-Ofelt intensity parameters Ω 2 , Ω 4 , and Ω 6 are obtained to be 6.76x10 -20 , 0.37x10 -20 , and 0.50x10 -20 cm 2 , respectively. Along crystallographic axes, refractive indices are presented. The fluorescence decay time of the 4 I 13/2 level has also been investigated and shows an exponential behavior with a lifetime value of 5.52 ms. The crystal is potentially used for green and infrared eye-safe lasers

Thermally stimulated luminescence in ZnMoO{sub 4} crystals

Energy Technology Data Exchange (ETDEWEB)

Degoda, V.Ya.; Kogut, Ya.P.; Moroz, I.M. [Kyiv National Taras Shevchenko University, MSP 03680 Kyiv (Ukraine); Danevich, F.A. [Institute for Nuclear Research, MSP 03680 Kyiv (Ukraine)

2017-03-15

Thermally stimulated luminescence in ZnMoO{sub 4} crystals after X-ray irradiation at temperatures 8 K, 85 K and 295 K was studied. A theoretical model of crystal phosphor with three types of traps (shallow, phosphorescent and deep) is proposed. Simple analytic solutions of the kinetic equations system describing localized electrons on the traps and holes on recombination centres were obtained by using approximations accepted in the classic theories of crystal phosphors. Analytical curves describing thermally stimulated luminescence were obtained. A substantial effect of the different traps concentrations ratios on the thermally stimulated luminescence and conductivity peaks shapes is shown. A good agreement of the theoretical curves with the experimental data for the thermally stimulated luminescence peak at 114 K is obtained.

Crystal structure of 4-allylsulfanyl-1H-pyrazolo[3,4-d]pyrimidine

Directory of Open Access Journals (Sweden)

Mohammed El Fal

2014-09-01

Full Text Available In the title compound, C8H8N4S, the pyrazolo[3,4-d]pyrimidine ring system is essentially planar, with a maximum deviation from the mean plane of 0.025 (3 Å. The allyl group is disordered over two sites in a 0.512 (6:0.488 (6 ratio. In the crystal, molecules are linked by pairs of N—H...N hydrogen bonds, forming inversion dimers with an R22(8 graph-set motif.

Na3Tb(PO4)2: Synthesis, crystal structure and greenish emitting properties

Science.gov (United States)

Zhao, Dan; Ma, Zhao; Liu, Bao-Zhong; Zhang, Rui-Juan; Wu, Zhi-Qiang; Wang, Jian; Duan, Pei-Gao

2018-03-01

A anhydrous orthoborate Na3Tb(PO4)2 has been prepared and its crystal structure was determined by X-Ray diffraction of a non-merohedral twinned single crystal. The results show that the compound crystallizes in monoclinic space group C2/c and the structure features a 3D framework containing PO4, NaO6, NaO7, NaO8 and TbO8 polyhedra. Under near-UV excitation (370 nm), Na3Tb(PO4)2 shows intense characteristic emission bands of Tb3+ (490 nm, 543 nm, 585 nm and 620 nm) with the CIE coordinate of (0.3062, 0.5901), corresponding to greenish color. The excitation spectrum covers a wide range from 340 nm to 390 nm, which indicates that phosphor Na3Tb(PO4)2 can be efficiently activated by near-UV LED ship.

Poly(methacrylic acid)-mediated morphosynthesis of PbWO4 micro-crystals

International Nuclear Information System (INIS)

Yu, J.G.; Zhao, X.F.; Liu, S.W.; Li, M.; Mann, S.; Ng, D.H.L.

2007-01-01

PbWO 4 crystals with various morphologies were fabricated via a facile poly(methacrylic acid)-mediated hydrothermal route. Novel microsized PbWO 4 single crystals with a needle-like shape as well as other morphologies, such as a fishbone, dendrite, sphere, spindle, ellipsoid, rod, and dumbbell with two dandelion-like heads, could be produced. The presence of PMAA, [Pb 2+ ]/[WO 4 2- ] molar ratio (R), and aging temperature played key roles in the formation of the PbWO 4 needle-like structures. Between temperatures of 60 to 150 C, the length and photoluminescence intensities of the PbWO 4 micro needles significantly increased with aging temperature, while the diameter did not change remarkably. Time-dependent experiments revealed that the formation of PbWO 4 microneedles involved an unusual growth process, involving nucleation, oriented assembly and controlled mesoscale restructuring of nanoparticle building blocks. (orig.)

Transport mean free path in K5Bi1-xNdx(MoO4)4 laser crystal powders

International Nuclear Information System (INIS)

Illarramendi, M A; Aramburu, I; Fernandez, J; Balda, R; Al-Saleh, M

2007-01-01

In this work, we calculate in two different ways the transport mean free paths in K 5 Bi 1-x Nd x (MoO 4 ) 4 (x = 0.05, 0.2, 1) laser crystal powders by using the diffuse spectral reflectance and transmittance of the powders and the absorption coefficient of the crystal materials. The theoretical calculations have been made by assuming a diffusive propagation of light in these materials. Similar results have been obtained from both methods

1H and 2H NMR relaxation study on the phase transitions of (NH4)3H(SO4)2 and (ND4)3D(SO4)2 single crystals

International Nuclear Information System (INIS)

Lim, Ae Ran; Jeong, Se-Young

2006-01-01

T 1 , T 1ρ and T 2 for the 1 H and 2 H nuclei in (NH 4 ) 3 H(SO 4 ) 2 and (ND 4 ) 3 D(SO 4 ) 2 single crystals grown using the slow evaporation method were measured for phases I, II, III, IV and V. The 1 H T 1 , T 1ρ , and T 2 values were found to exhibit different trends in phases II and III: T 1 , T 1ρ and T 2 for 1 H do not change significantly near the phase transition at 265 K, whereas near 413 K they change discontinuously. We conclude that the NH 4 + and H(SO 4 ) 2 - ions do not play an important role in the III-II phase transition, but do play important roles in the II-I phase transition. The liquid-like nature of the 1 H T 1ρ and T 2 above 413 K is indicative of the destruction and reconstruction of hydrogen bonds. Moreover, the phase transitions of the (NH 4 ) 3 H(SO 4 ) 2 crystal are accompanied by changes in the molecular motion of the (NH 4 ) + ions. The variations with temperature of the 2 H T 1 and T 2 of (ND 4 ) 3 D(SO 4 ) 2 crystals are not similar to those observed for the 1 H T 1 and T 2 . Our comparison of the results for (NH 4 ) 3 H(SO 4 ) 2 and (ND 4 ) 3 D(SO 4 ) 2 crystals indicates the following: the 1 H T 1ρ and T 2 of the (NH 4 ) + and H(SO 4 ) 2 - ions above T C1 are characteristic of fast, liquid-like motion, which is not the case for (ND 4 ) 3 D(SO 4 ) 2 ; and the 2 H T 1 of D(SO 4 ) 2 - in (ND 4 ) 3 D(SO 4 ) 2 is longer than the 2 H T 1 of (ND 4 ) + in contrast to the results for (NH 4 ) 3 H(SO 4 ) 2 crystals

Growth and optical properties of Tm:GdVO4 single crystal

International Nuclear Information System (INIS)

Urata, Y.; Akagawa, K.; Wada, S.; Tashiro, H.; Fukuda, T.

1999-01-01

Thulium-doped gadolinium vanadate (Tm:GdVO 4 ) single crystal has been successfully grown by a modified Czochralski (CZ) technique. Effective distribution coefficient of Tm was determined to be 0.74. Absorption characterization was performed in the 800 nm region and the maximum absorption peak was found at 799 nm for π polarization. Fluorescence spectra for tuning at the maximum absorption were obtained around 1.8-2.0 μm region with 100 nm bandwidth. This suggests that a Tm:GdVO 4 crystal is expected as a new promising LD pumped solid-state laser in the 2 μm region. (orig.)

Growth, crystal structure, spectral properties and laser performance of Yb3+:NaLu(MoO4)2 crystal

Science.gov (United States)

Yu, Yi; Zhang, Lizhen; Huang, Yisheng; Lin, Zhoubin; Wang, Guofu

2013-10-01

A double molybdate Yb3+:NaLu(MoO4)2 crystal was successfully grown from a flux of Na2Mo2O7 by the top-seeded solution growth method, for the first time to our knowledge. The crystal belongs to the tetragonal system with space group I41/a, and the unit-cell parameters are a = b = 5.159 Å, c = 11.246 Å. Na and Lu atoms co-occupy the same lattice site, which leads to the disordered structure of NaLu(MoO4)2 crystal. The thermal expansion coefficients of the crystal are 1.35 × 10-5 K-1 along the c-axis, and 1.01 × 10-5 K-1 along the a-axis. The full-width at half-maximum of the emission bands are 67 nm for the σ-polarization and 50 nm for the π-polarization at about 1020 nm. The maximum emission cross-sections for the σ- and π-polarizations are 2.79 × 10-20 cm2 and 2.94 × 10-20 cm2, respectively. 0.3 W output power at 1025 nm was obtained at an absorbed pump power of 1.7 W, with a slope efficiency of 24%.

Crystal structure of 4,4′-(ethane-1,2-diylbis(2,6-dibromoaniline

Directory of Open Access Journals (Sweden)

Ines Hauptvogel

2015-01-01

Full Text Available In the title compound, C14H12Br4N2, the molecule lies across an inversion center and hence the benzene rings are strictly coplanar. In the crystal, molecules are linked by N—H...N and weak N—H...Br hydrogen bonds, forming a two-dimensional network parallel to (101. In addition, type II Br...Br interactions [3.625 (4 Å] complete a three-dimensional supramolecular network.

Fundamental optical absorption edge in MnGa2Te4 single crystals

International Nuclear Information System (INIS)

Medvedkin, G.A.; Rud, Yu.V.; Tairov, M.A.

1988-01-01

A study is made of the optical properties of oriented MnGa 2 Te 4 crystals in the region of the fundamental absorption edge. The energy gap width for the temperatures 77, 300, and 370 K is determined to be E G = 1.635, 1.52, and 1.50 eV. The spectral response α(ℎω/2π) is found to follow Urbach's rule thoughout the temperature range studied, the slope of the absorption edge remaining constant (α = 10 2 cm -1 ). Crystal annealing with subsequent rapid cooling results in a shift of the absorption edge longward by 25 meV with the exponential form of α(ℎω/2π) prevailing over the range T = 77 to 370 K. An analysis shows the optical absorption in the region of the fundamental edge to be a sum of the effects coming from the density-of-states tails, local scattering centers associated with a high vacancy concentration, and electron-phonon interaction. Optical linear dichroism of the absorption edge of MnGa 2 Te 4 single crystals with pseudotetragonal structure is revealed and studied. The single crystals are established to be optically uniaxial, their optical transmission dichroism being negative. It is shown that the minimal direct optical transitions in MnGa 2 Te 4 are allowed in the E parallel c polarization in the temperature range 77 to 370 K, the crystal-field splitting of the valence band increasing with temperature. (author)

Growth, structural, optical, thermal and mechanical studies on 4-Aminopyridinium monophthalate: A novel nonlinear optical crystal

Science.gov (United States)

Marudhu, G.; Krishnan, S.; Palanichamy, M.

2016-03-01

A novel nonlinear optical crystal of 4-Aminopyridinium monophthalate (4-APMP) was grown by slow evaporation technique using methanol as solvent. Single crystal X-ray diffraction analysis confirms that the grown crystal belongs to orthorhombic system. The presence of functional groups was qualitatively determined by FTIR analysis. The optical absorption studies reveal very low absorption in the entire visible region. The fluorescence emission spectrum shows the emission is in blue region. The thermal stability of the grown crystal is found to be around 197.2 °C. The SHG efficiency of the grown crystal is found to be 1.1 times than that of KDP crystals.

Lanthanide 4f-level location in AVO4:Ln3+ (A = La, Gd, Lu) crystals

NARCIS (Netherlands)

Krumpel, A.H.; Van der Kolk, E.; Cavalli, E.; Boutinaud, P.; Bettinelli, M.; Dorenbos, P.

2009-01-01

The spectral properties of LaVO4, GdVO4 and LuVO4 crystals doped with Ce3+, Pr3+, Eu3+ or Tb3+ have been investigated in order to determine the position of the energy levels relative to the valence and conduction bands of the hosts along the trivalent and divalent lanthanide series. Pr3+ and Tb3+

Ultralong Lifespan and Ultrafast Li Storage: Single-Crystal LiFePO4 Nanomeshes.

Science.gov (United States)

Zhang, Yan; Zhang, Hui Juan; Feng, Yang Yang; Fang, Ling; Wang, Yu

2016-01-27

A novel LiFePO4 material, in the shape of a nanomesh, has been rationally designed and synthesized based on the low crystal-mismatch strategy. The LiFePO4 nanomesh possesses several advantages in morphology and crystal structure, including a mesoporous structure, its crystal orientation that is along the [010] direction, and a shortened Li-ion diffusion path. These properties are favorable for their application as cathode in Li-ion batteries, as these will accelerate the Li-ion diffusion rate, improve the Li-ion exchange between the LiFePO4 nanomesh and the electrolyte, and reduce the Li-ion capacitive behavior during Li intercalation. So the LiFePO4 nanomesh exhibits a high specific capacity, enhanced rate capability, and strengthened cyclability. The method developed here can also be extended to other similar systems, for instance, LiMnPO4 , LiCoPO4 , and LiNiPO4 , and may find more applications in the designed synthesis of functional materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Science.gov (United States)

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.

Pycnometric and Spectroscopic Studies of Red Phosphors Ca{sub (1-1.5x)}{sup 2+} WO{sub 4}:Eu{sub x}{sup 3+} Ca{sub (1}-{sub 2x)}{sup 2+} WO{sub 4}:Eu{sub x}{sup 3+},Na{sub x}{sup +}

Energy Technology Data Exchange (ETDEWEB)

Cho, Seonwoog [Silla Univ., Busan (Korea, Republic of)

2013-09-15

Red phosphors Ca{sub (1-1.5x)}Eu{sub x}WO{sub 4} and Ca{sub (1-2x)}Eu{sub x}Na{sub x}WO{sub 4} were synthesized with various concentrations x of Eu{sup 3+} ions by using a solid-state reaction method. The crystal structure of the red phosphors were found to be a tetragonal scheelite structure with space group I4{sub 1}/a. X-ray diffraction (XRD) results show the (112) main diffraction peak centered at 2θ = 28.71 .deg., and indicate that there is no basic structural deformation caused by the vacancies V{sub Ca}'' or the Eu{sup 3+} (and Na{sup +}) ions in the host crystals. Densities of Ca{sub (1.1.5x)}Eu{sub x}WO{sub 4} were measured on a (helium) gas pycnometer. Comparative results between the experimental and theoretical densities reveal that Eu{sup 3+} (and Na{sup +}) ions replace the Ca{sup 2+} ions in the host CaWO{sub 4}. Also, the photoluminescence (PL) emission and photoluminescence excitation (PLE) spectra show the optical properties of trivalent Eu{sup 3+} ions, not of divalent Eu{sup 2+}. Raman spectra exhibit that, without showing any difference before and after the doping of activators to the host material CaWO{sub 4}, all the gerade normal modes occur at the identical frequencies with the same shapes and weaker intensities after the substitution. However, the FT-IR spectra show that some of the ungerade normal modes have shifted positions and different shapes, caused by different masses of Eu{sup 3+} ions (or Na{sup +} ions, or V{sub Ca}'' vacancies) from Ca2{sup +}.

Synthesis, characterization and crystal structure of 6-Chloro-4,4‧-dimethyl-2,2‧-bipyridine and 4,4‧-Dimethyl 2,2‧-bipyridine N-Oxide

Science.gov (United States)

Conterosito, Eleonora; Magistris, Claudio; Barolo, Claudia; Croce, Gianluca; Milanesio, Marco

2016-03-01

The synthesis, the NMR characterization and the crystal structure of 6-Chloro 4,4‧-dimethyl 2,2‧-bipyridine and of the reaction intermediate 4,4‧-Dimethyl 2,2‧-bipyridine N-Oxide are here reported. The target compound crystallizes in the orthorhombic system while the intermediate is monoclinic. In both structures, the molecules are linked by weak interactions. The structure of the reaction intermediate N-oxide is characterized by a dihedral angle between the two phenyl rings of 161.77° while the other is almost planar with a dihedral angle of 179.15°. The crystal packing was investigated, also with the aid of Hirshfeld surface analysis. In the N-oxide reaction intermediate the packing is governed by CH-O interactions, while in the product the packing is simply driven by minimizing the voids and thus maximizing the density, with a prevalence of H•••H and C•••H contacts, as indicated by fingerprint decomposition analysis.

Acoustic anisotropy of acoustooptic TI(3)AsS(4) crystals.

Science.gov (United States)

Martynyuk-Lototska, Iryna; Kushnirevych, Marian; Zapeka, Bohdan; Krupych, Oleh; Kokhan, Oleksandr; Pogodin, Artem; Peresh, Eugen; Mys, Oksana; Vlokh, Rostyslav

2015-02-20

We present comprehensive experimental measurements and analysis of anisotropy of the acoustic wave velocities for TI(3)AsS(4) crystals, including the obliquity and nonorthogonality of the acoustic waves, and the deviations from purely longitudinal and transverse polarization types. We have found that the crystals under analysis are characterized by rather low transverse wave velocities v(23) and v(32), which are both equal to 630 m/s. It is shown that the efficiency of acoustooptic (AO) interactions in TI(3)AsS(4) can be notably increased when providing anisotropic interaction with the slowest transverse acoustic wave. Under the previously mentioned conditions, the AO figure-of-merit can be estimated to be extremely high, i.e., approximately 3×10(-12) s(3)/kg.

Crystal structure of molybdenyl tetrapolyphosphate (MoO)2P4O13

International Nuclear Information System (INIS)

Minacheva, L.Kh.; Antsishkina, A.S.; Lavrov, A.V.; Sakharova, V.G.; Nikolaev, V.P.; Poraj-Koshits, M.A.

1979-01-01

The structure of crystals of molybdenyl tetrapolyphosphate [MoO] 2 P 4 O 13 has been determined. The substance is crystallized in the monoclinic syngony with the following parameters of the elementary cell: a=8.288 (2); b=10.690 (3); c=19.529 (5) A; γ=106.7 (3) deg. The structural units are molybdenyl groups MoO(3 + ) and polyphosphate anions P 4 O 13 (6 - ) that are composed of four PO 4 tetrahedrons whose apexes are connected in series. Three atoms of phasphate anion form the ''internal'' P-O-P bridges, while the remaining oxygen atoms, the ''external'' P-O-Mo bridges. The optimum temperature of crystals synthesis is 450 - 460 deg C. A mixture of phase of MoO 2 P 4 O 13 and Mo(PO 3 ) 3 is obtained as temperature is raised up to 600 deg C. Consequently, the stepwise dissociation of molybdenyl ions with the splitting off of oxygen and gradual reduction in the degree of molybdenum oxidation (MoO 2 ) 2+ → (MoO) 3+ → Mo 3+ occurs in the solution

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

Science.gov (United States)

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.

Effects of composition modulation on the luminescence properties of Eu(3+) doped Li1-xAgxLu(MoO4)2 solid-solution phosphors.

Science.gov (United States)

Cheng, Fangrui; Xia, Zhiguo; Molokeev, Maxim S; Jing, Xiping

2015-11-07

Double molybdate scheelite-type solid-solution phosphors Li1-xAgxLu1-y(MoO4)2:yEu(3+) were synthesized by the solid state reaction method, and their crystal structures and luminescence properties were investigated in detail. The composition modulation and structural evolution of this series of samples were studied and the selected AgEu(MoO4)2, AgLu(MoO4)2, LiLu(MoO4)2 and LiEu(MoO4)2 phases were analyzed based on the Rietveld refinement. Depending on the variation of the Li/Ag ratio in Li1-xAgxLu1-y(MoO4)2:yEu(3+) phosphors, the difference in the luminescence properties of Li1-xAgxLu1-y(MoO4)2:yEu(3+) phosphors was ascribed to two factors, one reason could be assigned to the coupling effect and the nonradiative transition between the energy levels of LixAg1-xLu(MoO4)2 matrices and the activator Eu(3+), another could be due to the near ultraviolet energy absorption and transmission efficiency between the charge-transfer (CT) band of O(2-)-Mo(6+) and the 4f → 4f emissive transitions of Eu(3+). The ultraviolet-visible diffuse reflection spectra (UV-vis DRS) and Raman spectra analysis were also used to verify the above mechanism.

Synthesis, crystal growth, characterization and theoretical studies of 4-aminobenzophenonium picrate

Science.gov (United States)

Aditya Prasad, A.; Muthu, K.; Rajasekar, M.; Meenatchi, V.; Meenakshisundaram, S. P.

2015-01-01

Single crystals of 4-aminobenzophenonium picrate (4ABPP) were grown by slow evaporation of a mixed solvent system methanol-acetone (1:1,v/v) containing equimolar quantities of picric acid and 4-aminobenzophenone. The proton and carbon signals are confirmed by nuclear magnetic resonance spectroscopy. The various functional groups present in the molecule are identified by FT-IR analysis. Optimized geometry, first-order molecular hyperpolarizability (β), polarizability (α), bond length, bond angles and excited state energy from theoretical UV were derived by Hartree-Fock calculations. The complete assignment of the vibrational modes for 4-aminobenzophenonium picrate was performed by the scaled quantum mechanics force field (SQMFF) methodology using potential energy distribution. Natural bond orbital (NBO) calculations were employed to study the stabilities arising from charge delocalization and intermolecular interactions of 4ABPP. The atomic charge distributions of the various atoms present in 4ABPP are obtained by Mulliken charge population analysis. The as-grown crystal is further characterized by thermal and optical absorbance studies.

Crystal growth and magnetic properties of spinel (Co,Mn)3O4

Science.gov (United States)

Kang, Sun Hee; Kim, Ill Won; Jeong, Yoon Hee; Koo, Tae Yeong

2012-04-01

Single crystals of cubic and tetragonal spinel Co3-xMnxO4 (x=1.0 and 1.5) were successfully grown using a solvent evaporation method with PbF2 flux. Single crystals in octahedral shape with a size of about 4 mm on edge were obtained from 100 cm3 Pt crucibles. Ferrimagnetic transitions were detected at 170 K and 160 K from the measurements of temperature dependent magnetization and specific heat of Co2MnO4 and Co1.5Mn1.5O4, respectively. Low temperature field-dependent magnetization curves give a strong indication of the non-collinear spin structure, offering an insulating Co3-xMnxO4 system as a possible candidate for examining the multiferroicity.

Naturally occurring crystalline phases: analogues for radioactive waste forms

International Nuclear Information System (INIS)

Haaker, R.F.; Ewing, R.C.

1981-01-01

Naturally occurring mineral analogues to crystalline phases that are constituents of crystalline radioactive waste forms provide a basis for comparison by which the long-term stability of these phases may be estimated. The crystal structures and the crystal chemistry of the following natural analogues are presented: baddeleyite, hematite, nepheline; pollucite, scheelite;sodalite, spinel, apatite, monazite, uraninite, hollandite-priderite, perovskite, and zirconolite. For each phase in geochemistry, occurrence, alteration and radiation effects are described. A selected bibliography for each phase is included

Naturally occurring crystalline phases: analogues for radioactive waste forms

Energy Technology Data Exchange (ETDEWEB)

Haaker, R.F.; Ewing, R.C.

1981-01-01

Naturally occurring mineral analogues to crystalline phases that are constituents of crystalline radioactive waste forms provide a basis for comparison by which the long-term stability of these phases may be estimated. The crystal structures and the crystal chemistry of the following natural analogues are presented: baddeleyite, hematite, nepheline; pollucite, scheelite;sodalite, spinel, apatite, monazite, uraninite, hollandite-priderite, perovskite, and zirconolite. For each phase in geochemistry, occurrence, alteration and radiation effects are described. A selected bibliography for each phase is included.

Electron microprobe investigations of ore minerals of the Altenberg tin deposit (Erzgebirge, GDR). 3

International Nuclear Information System (INIS)

Foerster, H.J.; Hunger, H.J.; Grimm, L.

1987-01-01

Members of the scheelite-powellite solid solution series filling thin fractures or mantling wolframite were found in association with fluorite within a small polymineralic quartz vein traversing a topaz-protolithionite-quartz greisen. The composition of the mixed-crystal series determined by means of an automated ARL SEMQ energy-dispersive electron microprobe is characterized by a great variability and heterogeneity which has not previously been reported from any specimen nor from this special mode of occurrence yet. With an amount of powellite component between 3.2 and 58 mole percent, the molybdoscheelites from Altenberg show the today known extent of complete miscibility in the natural scheelite-powellite series. Final remarks deal with the possibilities of using the mineral series, together with some other tungsten minerals, as an indicator of the physicochemical conditions of ore formation. (author)

A Layered Solution Crystal Growth Technique and the Crystal Structure of (C 6H 5C 2H 4NH 3) 2PbCl 4

Science.gov (United States)

Mitzi, D. B.

1999-07-01

Single crystals of the organic-inorganic perovskite (C6H5C2H4NH3)2PbCl4 have been grown at room temperature using a layered solution approach. The bottom solution layer, contained within a long straight tube, consists of PbCl2 dissolved in concentrated aqueous HCl. A less dense layer of methanol is carefully placed on top of the HCl/PbCl2 solution using a syringe. Finally, a stoichiometric quantity of C6H5C2H4NH2 (relative to the PbCl2) is added to the top of the column. As the layers slowly diffuse together, well-formed crystals of (C6H5C2H4NH3)2PbCl4 appear near the interface between the HCl/PbCl2 and C6H5C2H4NH2 solutions. The thick, plate-like crystals are well suited for X-ray crystallography studies. Room temperature intensity data were refined using a triclinic (Poverline1) cell (a=11.1463(3) Å, b=11.2181(3) Å, c=17.6966(5) Å, α= 99.173(1)°, β=104.634(1)°, γ=89.999(1)°, V=2111.8(1) Å3, Z=4, Rf/Rw=0.031/0.044). The organic-inorganic layered perovskite structure features well-ordered sheets of corner-sharing distorted PbCl6 octahedra separated by bilayers of phenethylammonium cations. Tilting and rotation of the PbCl6 octahedra within the perovskite sheets, coupled with organic cation ordering, leads to the unusual in-sheet 2ap×2ap superstructure, where ap is the lattice constant for the ideal cubic perovskite.

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

Energy Technology Data Exchange (ETDEWEB)

Kumar, Sandeep; Andotra, Savit; Kaur, Mandeep [University of Jammu, Department of Chemistry (India); Gupta, Vivek K.; Kant, Rajni [Department of Physics and Electronics, University of Jammu, X-ray Crystallographic Laboratory (India); Pandey, Sushil K., E-mail: kpsushil@rediffmail.com [University of Jammu, Department of Chemistry (India)

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.

Investigation on optical band gap, photoluminescence properties and concentration quenching mechanism of Pb1 - x Tb3 +xWO4 green-emitting phosphors

Science.gov (United States)

Chanu, Thokchom Taru Taru; Rajmuhon Singh, N.

2018-02-01

A series of monophasic Tb3 + (2, 5, 7, 10 and 15 at%) doped PbWO4 phosphors were successfully prepared via hydrothermal method. X-ray diffraction patterns revealed that the prepared samples possess a high crystallinity with tetragonal scheelite-type structure. FT-IR and Raman analysis exhibited a Wsbnd O stretching peak of WO42 - group, which is also related to the scheelite structure. UV-visible diffuse reflectance spectra indicated a reduction in the optical band gap with the replacement of Pb2 + by Tb3 + ions. The presence of strong and intense emission peaks characteristic of Tb3 + with the dominant peak at 545 nm (green, 5D4 → 7F5 transition) under UV irradiation at 320 nm demonstrated an efficient energy transfer from the host to Tb3 + ions. Using Van Uitert's model, the concentration quenching mechanism between Tb3 + ions in PbWO4:Tb3 + phosphor was attributed to a dipole-dipole interaction and the critical distance was determined to be 12 Å. The decay lifetimes and CIE chromaticity co-ordinates of PbWO4:Tb3 + phosphors were also investigated in detail. These prepared materials might serve as a potential phosphor for LED applications.

Crystal growth, spectroscopic characterization, and continuous wave laser operation of Nd3+-doped LiLuF4 crystal

Science.gov (United States)

Zhao, C. C.; Hang, Y.; Zhang, L. H.; He, X. M.; Yin, J. G.; Li, R.; Yu, T.; Chen, W. B.

2011-04-01

Nd3+-doped LiLuF4 single crystal with high optical quality was grown by Czochralski technique. The segregation coefficient of Nd3+ in LiLuF4 crystal was determined by the inductively coupled plasma atomic emission spectrometry method. Polarized absorption and fluorescence spectra were investigated. The peak absorption cross section at 792 nm and peak emission cross section at 1053 nm are 6.94×10-20 and 7.60×10-20 cm2, respectively. With a laser-diode as the pump source, a maximum 6.22 W continuous-wave laser output at 1053 nm has been obtained with a slope efficiency of 37.2% with respect to the pump power.

On thermal expansion of RbD2PO4, CsH2PO4 and CsDrPO4 crystals

International Nuclear Information System (INIS)

Vlokh, O.G.; Shchur, Ya.I.; Klymiv, I.M.

1994-01-01

Thermal expansion of RbD 2 PO 4 , CsH 2 PO 4 , CsD 2 PO 4 crystals in a wide range of temperatures embracing points of phase transitions was studied. An explanation of anomalous behaviour of thermal expansion factor along directions b and c in the course of RbD 2 PO 4 transfer into intermediate phase was suggested. 10 refs., 4 figs

Monoclinic Paracetamol vs. Paracetamol-4,4′-Bipyridine Co-Crystal; What Is the Difference? A Charge Density Study

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Jonathan J. Du

2018-01-01

Full Text Available Paracetamol (PCM has two well-documented polymorphic forms at room temperature; monoclinic Form I is more stable than the other orthorhombic Form II. Form II exhibits improved tabletting properties compared to Form I due to low shearing forces; however, difficulties in its manufacture have limited its use in industrial manufacture. Previous studies have found that the introduction of a co-former to form co-crystals would allow the PCM molecule to exist in a conformation similar to that of the orthorhombic form while being more stable at room temperature. Experimental charge density analysis of the paracetamol-4,4′-bipyridine (PCM-44BP co-crystal system, and its constituent molecules, has been carried out to examine the forces that drive the formation and stabilisation of the co-crystal, while allowing PCM to maintain a packing motif similar to that found in Form II. It is hoped studies on this well-known compound will help apply the knowledge gained to other drug molecules that are less successful. The PCM molecules in the co-crystal were found to exhibit similar packing motifs to that found in Form I, however, intercalation of the 44BP molecule between the PCM layers resulted in a shallower angle between molecular planes, which could result in the required lateral shear. Topological analysis identified more weak interactions in the co-crystal compared to the individual molecules, thus allowing for greater stability as evidenced by the lattice energies. Weak interactions in the PCM-44BP co-crystal were found to range in strength from 4.08–84.33 kJ mol−1, and this variety allowed the PCM-44BP planes to be held together, while a weak π–π interaction (15.14 kJ mol−1 allowed lateral shear to occur, thus mimicking the planes found in Form II PCM and offering the possibility of improved tabletting properties. A comparison of integrated atomic charges between partitions of the PCM molecules in the single and co-crystal found that the

Growth, thermal and laser properties of Yb:YxLu1−xVO4 mixed crystal

International Nuclear Information System (INIS)

Zhong, Degao; Teng, Bing; Kong, Weijin; Li, Jianhong; Zhang, Shiming; Li, Yuyi; Cao, Lifeng; Yang, Liting; He, Linxiang; Huang, Wanxia

2015-01-01

New mixed crystal of Yb: Y 0.78 Lu 0.22 VO 4 with Yb ion concentration of 0.3 at% was grown by Czochralski method. Transmission synchrotron X-ray topography implies that this mixed crystal follows a rotational growth pattern. Crystal structure of this crystal was determined by X-ray diffraction. It showed that this crystal possesses a tetragonal zircon structure (ZrSiO 4 , space group I41/amd), as YVO 4 and LuVO 4 do. Thermal properties of this crystal were characterized by measuring its specific heat, thermal expansion coefficients and thermal conductivities. The specific heat was determined to be 0.500 J g −1 K −1 at 293 K. The average linear thermal expansion coefficients were calculated to be α 11 = 1.73 × 10 −6 K −1 and α 33 = 9.43 × 10 −6 K −1 , over the temperature range of 300–777 K. The thermal conductivities were calculated to be κ 11 = 5.47 W m −1 K −1 and κ 33 = 6.64 W m −1 K −1 at 303 K. Continuous-wave (cw) laser test on Yb: Y 0.78 Lu 0.22 VO 4 was conducted at room temperature in the wavelength range of 1035.7–1048.3 nm, and a 13.5% optical-to-optical efficiency was achieved. The good thermal properties of Yb:Y 0.78 Lu 0.22 VO 4 mixed crystal and its attractive cw laser performance make it very suitable for practical applications. - Highlights: • New Yb:Y 0.78 Lu 0.22 VO 4 mixed laser crystals were grown. • The thermal expansion, thermal diffusivity and specific heat were measured. • Cw laser operation was realized at room temperature in the range of 1035.7–1048.3 nm

Study of gel grown mixed crystals of Bax Ca ((IO3) 4

Indian Academy of Sciences (India)

The growth of mixed crystals of BaCa1–(IO3)4 were carried out with simple gel method. The effect of various parameters such as pH of gel solution, gel concentration, gel setting time, concentration of reactants on the growth was studied. Crystals having different morphologies and habits were obtained. The grown ...

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

Science.gov (United States)

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.

Crystal structures and magnetic properties of iron (III)-based phosphates: Na4NiFe(PO4)3 and Na2Ni2Fe(PO4)3

International Nuclear Information System (INIS)

Essehli, Rachid; Bali, Brahim El; Benmokhtar, Said; Bouziane, Khalid; Manoun, Bouchaib; Abdalslam, Mouner Ahmed; Ehrenberg, Helmut

2011-01-01

Graphical abstract: A perspective view of the Na 2 Ni 2 Fe(PO 4 ) 3 structure along the [0 0 1] direction. Both compounds seem to exibit antiferromagnetic interactions between magnetic entities at low temperature. Display Omitted Research highlights: → Nasicon and Alluaudite compounds, Iron(III)-based phosphates, Crystal structures of Na 4 NiFe(PO 4 ) 3 and Na 2 Ni 2 Fe(PO 4 ) 3 . → Magnetism behaviours of Na 4 NiFe(PO 4 ) 3 and Na 2 Ni 2 Fe(PO 4 ) 3 . → Antiferromagnetism interactions. → Mossbauer spectroscopy. - Abstract: Crystal structures from two new phosphates Na 4 NiFe(PO 4 ) 3 (I) and Na 2 Ni 2 Fe(PO 4 ) 3 (II) have been determined by single crystal X-ray diffraction analysis. Compound (I) crystallizes in a rhombohedral system (S. G: R-3c, Z = 6, a = 8.7350(9) A, c = 21.643(4) A, R 1 = 0.041, wR 2 =0.120). Compound (II) crystallizes in a monoclinic system (S. G: C2/c, Z = 4, a = 11.729(7) A, b = 12.433(5) A, c = 6.431(2) A, β = 113.66(4) o , R 1 = 0.043, wR 2 =0.111). The three-dimensional structure of (I) is closely related to the Nasicon structural type, consisting of corner sharing [(Ni/Fe)O 6 ] octahedra and [PO 4 ] tetrahedra forming [NiFe(PO 4 ) 3 ] 4+ units which align in chains along the c-axis. The Na + cations fill up trigonal antiprismatic sites within these chains. The crystal structure of (II) belongs to the alluaudite type. Its open framework results from [Ni 2 O 10 ] units of edge-sharing [NiO 6 ] octahedra, which alternate with [FeO 6 ] octahedra that form infinite chains. Coordination of these chains yields two distinct tunnels in which site Na + . The magnetization data of compound (I) reveal antiferromagnetic (AFM) interactions by the onset of deviations from a Curie-Weiss behaviour at low temperature as confirmed by Moessbauer measurements performed at 4.2 K. The corresponding temperature dependence of the reciprocal susceptibility χ -1 follows a typical Curie-Weiss behaviour for T > 105 K. A canted AFM state is proposed for

Crystal structure of [propane-1,3-diylbis(piperidine-4,1-diyl]bis[(pyridin-4-ylmethanone]–4,4′-oxydibenzoic acid (1/1

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Emily M. Low

2014-09-01

Full Text Available In the title co-crystal, C25H32N4O2·C14H10O5, molecules are connected into supramolecular chains aligned along [102] by O—H...N hydrogen bonding. These aggregate into supramolecular layers oriented parallel to (20-1 by C—H...O interactions. These layers then stack in an ABAB pattern along the c crystal direction to give the full three-dimensional crystal structure. The central chain in the dipyridylamide has an anti–anti conformation. The dihedral angle between the aromatic ring planes is 29.96 (3°. Disorder is noted in some of the residues in the structure and this is manifested in two coplanar dispositions of one statistically disordered carboxylic acid group.

The crystal structure of bøgvadite (Na2SrBa2Al4F20)

DEFF Research Database (Denmark)

Balic Zunic, Tonci

2014-01-01

The crystal structure of bøgvadite, Na2SrBa2Al4F20, has been solved and refined to a R1 factor of 4.4% from single-crystal data (MoKα X-ray diffraction, CCD area detector) on a sample from the cryolite deposit at Ivittuut, SW Greenland. Bøgvadite is monoclinic, P21/n space group, with unit cell...... parameters a= 7.134(1), b= 19.996(3) and c= 5.3440(8) Å, β = 90.02(1)o. A close proximity of the crystal structure to an orthorhombic symmetry and the presence of the two twin components in a nearly 1:1 ratio suggest that the investigated bøgvadite crystal has originally formed as a high......-temperature orthorhombic polymorph which on cooling transformed to the stable low temperature monoclinic structure. The bøgvadite crystal structure has groupings of cation-fluoride coordination polyhedra similar to those found in the crystal structures of the genetically closely associated minerals jarlite...

Structural, optical and electronic properties of K2Ba(NO3)4 crystal

Science.gov (United States)

Isaenko, L. I.; Korzhneva, K. E.; Goryainov, S. V.; Goloshumova, A. A.; Sheludyakova, L. A.; Bekenev, V. L.; Khyzhun, O. Y.

2018-02-01

Nitrate crystals reveal nonlinear optical properties and could be considered as converters of laser radiation in the short-wave region. The conditions for obtaining and basic properties of K2Ba(NO3)4 double nitrate crystals were investigated. Crystal growth was implemented by slow cooling in the temperature range of 72-49 °C and low rate evaporation. The structural analysis of K2Ba(NO3)4 formation on the basis of two mixed simple nitrate structures is discussed. The main groups of oscillations in K2Ba(NO3)4 crystal were revealed using Raman and IR spectroscopy, and the table of vibrations for this compound was compiled. The electronic structure of K2Ba(NO3)4 was elucidated in the present work from both experimental and theoretical viewpoints. In particular, X-ray photoelectron spectroscopy (XPS) was employed in the present work to measure binding energies of the atoms constituting the titled compound and its XPS valence-band spectrum for both pristine and Ar+ ion-bombarded surfaces. Further, total and partial densities of states of constituent atoms of K2Ba(NO3)4 have been calculated. The calculations reveal that the O 2p states dominate in the total valence-band region of K2Ba(NO3)4 except of its bottom, where K 3p and Ba 5p states are the principal contributors, while the bottom of the conduction band is composed mainly of the unoccupied O 2p states, with somewhat smaller contributions of the N 2p∗ states as well. With respect to the occupation of the valence band by the O 2p states, the present band-structure calculations are confirmed by comparison on a common energy scale of the XPS valence-band spectrum and the X-ray emission O Kα band for the K2Ba(NO3)4 crystal under study. Furthermore, the present calculations indicate that the K2Ba(NO3)4 compound is a direct-gap material.

Ultraviolet laser-induced voltages in LaSrAlO4 single crystal

International Nuclear Information System (INIS)

Zhi-Qing, Lü; Kun, Zhao; Song-Qing, Zhao; Hui, Zhao; Qing-Li, Zhou

2009-01-01

Laser-induced ultrafast photovoltaic effect is observed in LaSrAlO 4 single crystal at ambient temperature without any applied bias. An open-circuit photovoltage is obtained when the wafer is irradiated by a 248-nm-KrF laser pulse of 20 ns duration. The response time and full width at half maximum of the photovoltage pulse are 6 ns and 19 ns, respectively, indicating that LaSrAlO 4 single crystal has potential application in ultraviolet detector. (condensed matter: electronic structure, electrical, magnetic, and optical properties)

Synthesis and Crystal Structure of 1-Chloro-2-methyl-4-nitrobenzene

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Jim Simpson

2012-03-01

Full Text Available The title compound (3 was prepared from 4-chloroaniline in good yield on successive oxidation and methylation and its crystal and molecular structure is reported. The compound crystallizes in the monoclinic space group P 21/n with unit cell dimensions a = 13.5698(8, b = 3.7195 (3, c = 13.5967 (8 Å, ß = 91.703(3 °, V = 685.96 (10 Å3. The molecule is essentially planar with a dihedral angle of 6.2(3 ° between the nitro group and the phenyl ring. The crystal structure is stabilised by π...π contacts between adjacent benzene rings together with C–H...O hydrogen bonds and close Cl...O contacts.

Synthesis and crystal structure of the cesium silver permanganate Cs{sub 3}Ag[MnO{sub 4}]{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Bauchert, Joerg M.; Henning, Harald; Schleid, Thomas [Institut fuer Anorganische Chemie, Universitaet Stuttgart (Germany)

2012-09-15

After successful syntheses and structural refinements of the already known permanganates of cesium (Cs[MnO{sub 4}]) and silver (Ag[MnO{sub 4}]) we started to blend aqueous solutions of both components in various molar ratios. From crystallization experiments of these mixtures only three species of crystals with different chemical compositions were obtained: tricesium monosilver tetrakispermanganate (Cs{sub 3}Ag[MnO{sub 4}]{sub 4}) and, depending upon the respective ratio, either additional silver permanganate or surplus cesium permanganate, namely. The new title compound crystallizes in the orthorhombic space group Pnnm (no. 58) with two formula units per unit cell and cell dimensions of a = 764.53(4), b = 1883.57(9) and c = 584.34(3) pm. The crystal structure of Cs{sub 3}Ag[MnO{sub 4}]{sub 4} consists of two crystallographically distinguishable cesium cations. (Cs1){sup +} is surrounded by fourteen oxygen atoms constructing a slightly distorted bicapped hexagonal prism. These polyhedra are connected through edge-sharing with two other polyhedra of this kind to form chains along [001]. The chains are linked to each other via sixfold coordinated Ag{sup +} cations (d(Ag-O) = 238-246 pm), arranged in such a manner that they link three oxygen atoms of two cesium polyhedra, leading to a two-dimensional layer spreading out parallel to the (001) plane. Together with the two crystallographically different tetrahedral oxomanganate(VII) anions [MnO{sub 4}]{sup -} (d(Mn-O) = 161-162 pm) the other kind of cesium cations ((Cs2){sup +} with CN = 13) finally connect these layers three-dimensionally. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Modulated crystal structures of VII and V phases in (NH4)3H(SO4)2. I. Neutron Laue diffraction

International Nuclear Information System (INIS)

McIntyre, G.; Smirnov, L.S.; Baranov, A.I.; Dolbinina, V.V.; Frontas'eva, M.V.; Pavlov, S.S.; Pankratova, Yu.S.

2010-01-01

The study of crystal structures of VII and V phases of (NH 4 ) 3 H(SO 4 ) 2 by means of neutron Laue diffraction is carried out at temperatures from 5 to 300 K. It is found that crystal structures of VII and V phases have incommensurate modulation with different periods, and phase transition from phase VII to phase V is transition of the first type

Blue luminescence in Tm3+-doped KGd(WO4)2 single crystals

International Nuclear Information System (INIS)

Gueell, F.; Mateos, X.; Gavalda, Jna.; Sole, R.; Aguilo, M.; Diaz, F.; Massons, J.

2004-01-01

Up-conversion blue emissions of trivalent thulium ions in monoclinic KGd(WO 4 ) 2 single crystals at 454 and 479 nm are reported for a single pump laser source at 688 nm. We grew thulium-doped KGd(WO 4 ) 2 single crystals at several concentrations from 0.1% to 10%. We recorded a polarized optical absorption spectrum for the 3 F 2 + 3 F 3 energy levels of thulium at room temperature and low temperature (6 K). From the low temperature emission spectra we determined the splitting of the 3 H 6 ground state. The blue emissions are characterized as a function of the dopant concentration and temperature from 10 K to room temperature. To our knowledge, this is the first time that sequential two-photon excitation process (STEP) generated blue emissions in thulium-doped single crystals with a single excitation wavelength

Conformity Check of Thickness to the Crystal Plate λ/4(λ/2

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Alexander Syuy

2013-01-01

Full Text Available This work demonstrates that if crystal plates are identical in thickness in the direction of radiation, the intensity at the output of the polarizer-crystal-crystal-analyzer system equals zero. This means that it is possible to control the difference in thickness between the reference crystal plate (e.g., plates of λ/4 or λ/2 and the examined plate by the intensity of the transmitted radiation. Further, it shows that if nonmonochromatic radiation is used, then the spectrum of radiation at the output is determined by the relative orientation of the optical elements and their sizes. The paper gives the theoretical model for calculations of profile of spectra for the number of important cases of orientation of elements.

Europium doping in monoclinic KYb(WO{sub 4}){sub 2} crystal

Energy Technology Data Exchange (ETDEWEB)

Loiko, P.A. [Física i Cristallografia de Materials i Nanomaterials (FiCMA-FiCNA), Universitat Rovira i Virgili (URV), Campus Sescelades, c/ Marcellí Domingo, s/n., Tarragona, Spain E-43007 (Spain); Center for Optical Materials and Technologies (COMT), Belarusian National Technical University, 65/17 Nezavisimosti Ave., Minsk 220013 (Belarus); Vilejshikova, E.V. [Center for Optical Materials and Technologies (COMT), Belarusian National Technical University, 65/17 Nezavisimosti Ave., Minsk 220013 (Belarus); Mateos, X., E-mail: xavier.mateos@urv.cat [Física i Cristallografia de Materials i Nanomaterials (FiCMA-FiCNA), Universitat Rovira i Virgili (URV), Campus Sescelades, c/ Marcellí Domingo, s/n., Tarragona, Spain E-43007 (Spain); Serres, J.M. [Física i Cristallografia de Materials i Nanomaterials (FiCMA-FiCNA), Universitat Rovira i Virgili (URV), Campus Sescelades, c/ Marcellí Domingo, s/n., Tarragona, Spain E-43007 (Spain); Dunina, E.B.; Kornienko, A.A. [Vitebsk State Technological University, 72 Moskovskaya Ave., Vitebsk 210035 (Belarus); Yumashev, K.V. [Center for Optical Materials and Technologies (COMT), Belarusian National Technical University, 65/17 Nezavisimosti Ave., Minsk 220013 (Belarus); Aguiló, M.; Díaz, F. [Física i Cristallografia de Materials i Nanomaterials (FiCMA-FiCNA), Universitat Rovira i Virgili (URV), Campus Sescelades, c/ Marcellí Domingo, s/n., Tarragona, Spain E-43007 (Spain)

2017-03-15

We report on a detailed spectroscopic study of Eu{sup 3+} ions in the monoclinic KYb(WO{sub 4}){sub 2} crystal. The polarized room and low-temperature absorption spectra are measured. The maximum σ{sub abs} corresponding to the {sup 7}F{sub 1} → {sup 5}D{sub 1} transition is 1.32×10{sup –20} cm{sup 2} at 534.2 nm with a bandwidth of 0.7 nm (for E||N{sub m}). The Stark sub-levels of the excited mulitplets are determined. A Judd-Ofelt analysis is applied to the Eu{sup 3+}:KYb(WO{sub 4}){sub 2} crystal to determine the probability of spontaneous transitions, radiative lifetimes and luminescence branching ratios. Within the strong configuration interaction (SCI) approximation, the intensity parameters are Ω{sub 2}=4.757, Ω{sub 4}=2.295, Ω{sub 6}=1.644 [10{sup –20} cm{sup 2}] and Δ{sub f}=50160 cm{sup –1}. The radiative lifetime of the {sup 5}D{sub 0} state is 351 µs. The maximum stimulated-emission cross-section corresponding to the {sup 7}F{sub 1} → {sup 5}D{sub 1} transition is 1.44×10{sup –20} cm{sup 2} at 703.2 nm (for E||N{sub m}). Under UV excitation, the Eu{sup 3+}:KYb(WO{sub 4}){sub 2} crystal provides intense red photoluminescence with CIE coordinates, x=0.675, y=0.325.

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

Energy Technology Data Exchange (ETDEWEB)

Makarova, I. P., E-mail: makarova@crys.ras.ru; Grebenev, V. V.; Komornikov, V. A.; Selezneva, E. V. [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics,” (Russian Federation)

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.

Growth and laser characterization of a mixed laser crystal Nd: Lu 0.141Y 0.855VO 4

Science.gov (United States)

Zhao, Bin; Zhuang, Naifeng; Li, Tao; Guo, Feiyun; Zhuo, Zhuang; Ye, Jing; Chen, Jianzhong

2011-11-01

A new Nd: Lu 0.141Y 0.855VO 4 mixed laser crystal had been successfully grown by the Czochralski method. The reason of the crystal boule appearing additionally yellowish at the bottom was discussed. The X-ray powder diffraction analysis showed that the as-grown mixed crystal possesses the ZrSiO 4 structure. The effective segregation coefficients of Nd 3+ and Lu 3+ ions in the crystal were measured to be about 0.51 and 0.76, respectively. The room temperature fluorescence spectrum of the mixed crystal showed that the FWHM (full-width at half-maximum) of the 1064.9 nm fluorescence band was 5.1 nm, broader than that of Nd: YVO 4. A continuous-wave (CW) laser output was achieved with the Nd: Lu 0.141Y 0.855VO 4 crystal at 1.06 μm using laser diode pumping. The maximum CW output power of 1.7 W was obtained with the pump power of 7.6 W, higher than the 1.38 W achieved with the 0.5 at% Nd: LuVO 4 crystal under the same experimental conditions. All the results above show that the Nd: Lu 0.141Y 0.855VO 4 crystal is a promising laser material.

Growth and laser characterization of mixed Nd:Lu xGd 1-xVO 4 laser crystals

Science.gov (United States)

Yu, Haohai; Yu, Yonggui; Zhang, Huaijin; Wang, Zhengping; Wang, Jiyang; Cheng, Xiufeng; Shao, Zongshu; Jiang, Minhua

2006-08-01

A new series Nd:Lu xGd 1-xVO 4 ( x=0.14, 0.32, 0.50, 0.61, 0.70 and 0.80) mixed laser crystals have been successfully grown by the Czochralski method. The X-ray powder diffraction (XRPD) analysis shows that the as-grown mixed crystals possess the ZrSiO 4 structure. The cell parameters are found to decrease with an increase of x. The optical absorption spectra of the mixed crystals have been measured at room temperature, and five strong-absorption bands centered at the wavelengths of 531, 594, 752, 807 and 880 nm have been revealed in all crystals. They are assigned to the different spin- and electric-dipole-allowed transition from the ground state to the 2K 13/2+ 4G 7/2+ 4G 9/2, 4G 5/2+ 2G 7/2, 4F 7/2+ 4S 3/2, 4F 5/2+ 2H 9/2 and 4F 3/2 energy levels, respectively. A continuous-wave (CW) laser output has been achieved with the mixed crystals at 1.06 μm under laser diode pumping. The maximum CW output power of 377.4 mW has been obtained with the pump power of 2 W, and the corresponding optical conversion efficiency is 18.8%.

Trace elements determination in tungsten ores by neutron activation analysis

International Nuclear Information System (INIS)

Mireles Garcia, F.

1991-01-01

The kinetics approach of the leaching of industrial scheelite (CaWO 4 ) concentrates in hydrochloric acid media investigated under controlled acid concentration in leachates, reaction atmospheres and temperature conditions. Experiments show that the scheelite decomposition rate increases as the acid concentration in the leaching solution and temperature increase. The apparent activation energy for the scheelite acid decomposition process is estimated in the present study to be equal to 10.43 Kcal(mol) -1 . On the basis of the experimental results, it is proposed an equilibria competition mechanism as a function of the acid concentration which explains the peculiar behavior of the experimental systems at low temperatures. (Author)

Crystal field parameters in UCl/sub 4/: Experiment versus theory

Energy Technology Data Exchange (ETDEWEB)

Zolnierek, Z.; Gajek, Z. (Polska Akademia Nauk, Wroclaw. Inst. Niskich Temperatur i Badan Strukturalnych); Khan Malek, C. (Paris-11 Univ., 91 - Orsay (France). Inst. de Physique Nucleaire)

1984-08-01

Crystal field effect on U/sup 4 +/ ion with the /sup 3/H/sub 4/ ground term in tetragonal ligand field of UCl/sub 4/ has been studied in detail. Crystal field parameters determined experimentally from optical spectroscopy and magnetic susceptibility are in good agreement with CEP sets derived from the modified point charge model and the ab initio method. Theoretical calculations lead to overestimating the A/sub 4//sup 4/4/> and lowering the A/sub 2//sup 0/ values in comparison to those found in the experiments. The discrepancies are, however, within an accuracy of calculations. A large similar reduction of expectation values of the magnetic moment operator for the eigenvectors of lowest CF levels (17.8%), determined from magnetic susceptibility, cannot be attributed to the overlap and covalency effects only. The detailed calculations have shown that the latter effects provide about 4.6% reduction of respective matrix elements, and the applied J-J mixing procedure increases this factor up to 6.5%. Since similar reduction factor has already been observed in a number of different uranium compounds, as in UCl/sub 4/ it seems to be likely that this feature is involved in the intrinsic properties of the U/sup 4 +/ ion. The authors endeavor to explain this effect in terms of configuration interaction mechanisms.

Optical diagnostics of lead and PbGa2S4 layered crystal laser plasmas

International Nuclear Information System (INIS)

Shuaibov, A.K.; Dashchenko, A.I.; Shevera, I.V.

2001-01-01

Laser plasmas produced at the surfaces of lead and a PbGa 2 S 4 layered crystal irradiated by a neodymium laser with λ = 1.06 μm, pulse duration τ = 20 ns, and intensity W = (1-2) x 10 9 W/cm 2 are studied using optical diagnostics. It is shown that, in a lead plasma, the most intense (characteristic) lines are the PbI 405.7-nm, PbI 368.3-nm, PbI 364-nm, and PbII 220.4-nm lines. In a layered crystal plasma, the emission spectrum is an aggregation of the most intense PbI and GaI lines, whereas sulfur lines are absent. The bottlenecks of the recombination of the ionic and atomic components of the lead and PbGa 2 S 4 crystal plasmas are determined. The average propagation velocity of the lead laser plume is 18-20 km/s. A comparative analysis of the emission dynamics of PbI and GaI lines in the laser plasmas of these metals and in the plasma of a PbGa 2 S 4 crystal is carried out. The results obtained are important for the optical diagnostics of the plasmas of lead- and gallium-containing crystals and for the optimization of laser deposition of the thin films of these substances

Calcium Sulfoaluminate Sodalite (Ca 4 Al 6 O 12 SO 4 ) Crystal Structure Evaluation and Bulk Modulus Determination

KAUST Repository

Hargis, Craig W.; Moon, Juhyuk; Lothenbach, Barbara; Winnefeld, Frank; Wenk, Hans-Rudolf; Monteiro, Paulo J. M.

2013-01-01

The predominant phase of calcium sulfoaluminate cement, Ca 4(Al6O12)SO4, was investigated using high-pressure synchrotron X-ray diffraction from ambient pressure to 4.75 GPa. A critical review of the crystal structure of Ca4(Al 6O12)SO4 is presented

Neutral coordination polymers based on a metal-mono(dithiolene) complex: synthesis, crystal structure and supramolecular chemistry of [Zn(dmit)(4,4'-bpy)]n, [Zn(dmit)(4,4'-bpe)]n and [Zn(dmit)(bix)]n (4,4'-bpy = 4,4'-bipyridine, 4,4'-bpe = trans-1,2-bis(4-pyridyl)ethene, bix = 1,4-bis(imidazole-1-ylmethyl)-benzene.

Science.gov (United States)

Madhu, Vedichi; Das, Samar K

2011-12-28

This article describes a unique synthetic route that enables a neutral mono(dithiolene)metal unit, {Zn(dmit)}, to link with three different organic molecules, resulting in the isolation of a new class of neutral coordination polymers. The species {Zn(dmit)} coordinates with 4,4'-bipyridine (4,4'-bpy), trans-1,2-bis(4-pyridyl)ethene (4,4'-bpe) and 1,4-bis(imidazole-1-ylmethyl)-benzene (bix) as linkers giving rise to the formation of coordination polymers [Zn(dmit)(4,4'-bpy)](n) (1), [Zn(dmit)(4,4'-bpe)](n) (2) and [Zn(dmit)(bix)](n) (3) respectively. Compounds 1-3 were characterized by elemental analyses, IR, diffuse reflectance and single crystal X-ray diffraction studies. Compounds 1 and 3 crystallize in the monoclinic space group P2(1)/n, whereby compound 2 crystallizes in triclinic space group P1[combining macron]. In the present study, we chose three linkers 4,4'-bpy, 4,4'-bpe and bix (see , respectively, for their structural drawings), that differ in terms of their molecular dimensions. The crystal structures of compounds 1-3 are described here in terms of their supramolecular diversities that include π-π interactions, not only among aromatic stacking (compounds 1 and 3), but also between an aromatic ring and an ethylenic double bond (compound 2). The electronic absorption spectroscopy of compounds 1-3 support these intermolecular π-π interactions. This journal is © The Royal Society of Chemistry 2011

Crystallization and Preliminary X-ray Analysis of Bacteriophasge T4 UvsY Recombination Mediator Protein

International Nuclear Information System (INIS)

Xu, H.; Beernink, H.; Rould, M.; Morrical, S.

2006-01-01

Bacteriophage T4 UvsY protein is considered to be the prototype of recombination mediator proteins, a class of proteins which assist in the loading of recombinases onto DNA. Wild-type and Se-substituted UvsY protein have been expressed and purified and crystallized by hanging-drop vapor diffusion. The crystals diffract to 2.4 (angstrom) using in-house facilities and to 2.2 (angstrom) at NSLS, Brookhaven National Laboratory. The crystals belong to space group P422, P4 2 22, P42 1 2 or P4 2 2 1 2, the ambiguity arising from pseudo-centering, with unit-cell parameters a = b = 76.93, c = 269.8 (angstrom). Previous biophysical characterization of UvsY indicates that it exists primarily as a hexamer in solution. Along with the absence of a crystallographic threefold, this suggests that the asymmetric unit of these crystals is likely to contain either three monomers, giving a solvent content of 71%, or six monomers, giving a solvent content of 41%

Granite-related Yangjiashan tungsten deposit, southern China

Science.gov (United States)

Xie, Guiqing; Mao, Jingwen; Li, Wei; Fu, Bin; Zhang, Zhiyuan

2018-04-01

The Yangjiashan scheelite-bearing deposit (38,663 metric tons of WO3 with an average ore grade of 0.70% WO3) is hosted in quartz veins in a biotite monzogranite intrusion and surrounding slate in the Xiangzhong Metallogenic Province of southern China. The monzogranite has a zircon SHRIMP U-Pb age of 406.6 ± 2.8 Ma (2σ, n = 20, MSWD = 1.4). Cassiterite coexisting with scheelite yields a weighted mean 206Pb/238U age of 409.8 ± 5.9 Ma (2σ, n = 30, MSWD = 0.20), and molybdenite intergrown with scheelite yields a weighted mean Re-Os age of 404.2 ± 3.2 Ma (2σ, n = 3, MSWD = 0.10). These results suggest that the Yangjiashan tungsten deposit is temporally related to the Devonian intrusion. The δD and calculated δ18OH2O values of quartz intergrown with scheelite range from - 87 to - 68‰, and - 1.2 to 3.4‰, respectively. Sulfides have a narrow range of δ34S values of - 2.9 to - 0.7‰ with an average value of - 1.6‰ (n = 16). The integration of geological, stable isotope, and geochronological data, combined with the quartz-muscovite greisen style of ore, supports a magmatic-hydrothermal origin for the tungsten mineralization. Compared to the more common tungsten skarn, quartz-wolframite vein, and porphyry tungsten deposits, as well as orogenic gold deposits worldwide, the Yangjiashan tungsten deposit is an unusual example of a granite-related, gold-poor, scheelite-bearing quartz vein type of deposit. The calcium needed for the formation of scheelite is derived from the sericitization of calcic plagioclase in the monzogranite and Ca-bearing psammitic country rocks, and the relatively high pH, reduced and Ca-rich mineralizing fluid may be the main reasons for the formation of scheelite rather than wolframite at Yangjiashan.

Actual and Idealized Crystal Field Parameterizations for the Uranium Ions in UF 4

Science.gov (United States)

Gajek, Z.; Mulak, J.; Krupa, J. C.

1993-12-01

The crystal field parameters for the actual coordination symmetries of the uranium ions in UF 4, C2 and C1, and for their idealizations to D2, C2 v , D4, D4 d , and the Archimedean antiprism point symmetries are given. They have been calculated by means of both the perturbative ab initio model and the angular overlap model and are referenced to the recent results fitted by Carnall's group. The equivalency of some different sets of parameters has been verified with the standardization procedure. The adequacy of several idealized approaches has been tested by comparison of the corresponding splitting patterns of the 3H 4 ground state. Our results support the parameterization given by Carnall. Furthermore, the parameterization of the crystal field potential and the splitting diagram for the symmetryless uranium ion U( C1) are given. Having at our disposal the crystal field splittings for the two kinds of uranium ions in UF 4, U( C2) and U( C1), we calculate the model plots of the paramagnetic susceptibility χ( T) and the magnetic entropy associated with the Schottky anomaly Δ S( T) for UF 4.

Synthesis, antityrosinase activity of curcumin analogues, and crystal structure of (1E,4E)-1,5-bis(4-ethoxyphenyl)penta-1,4-dien-3-one

Energy Technology Data Exchange (ETDEWEB)

Chantrapromma, S., E-mail: suchada.c@psu.ac.th; Ruanwas, P. [Prince of Songkla University, Department of Chemistry, Faculty of Science (Thailand); Boonnak, N. [Thaksin University, Department of Basic Science and Mathematics, Faculty of Science (Thailand); Chantrapromma, K. [Hatyai University, Faculty of Science and Technology (Thailand); Fun, H.-K. [Universiti Sains Malaysia, X-ray Crystallography Unit, School of Physics (Malaysia)

2016-12-15

Five derivatives of curcumin analogue (R = OCH{sub 2}CH{sub 3} (1), R = N(CH{sub 3}){sub 2} (2), R = 2,4,5-OCH{sub 3} (3), R = 2,4,6-OCH{sub 3} (4), and R = 3,4,5-OCH{sub 3} (5)) were synthesized and characterized by {sup 1}H NMR, FT-IR and UV–Vis spectroscopy. The synthesized derivatives were screened for antityrosinase activity, and found that 4 and 5 possess such activity. The crystal structure of 1 was determined by single crystal X-ray diffraction: monoclinic, sp. gr. P2{sub 1}/c, a = 17.5728(15) Å, b = 5.9121(5) Å, c = 19.8269(13) Å, β = 121.155(5)°, Z = 4. The molecule 1 is twisted with the dihedral angle between two phenyl rings being 15.68(10)°. In the crystal packing, the molecules 1 are linked into chains by C−H···π interactions and further stacked by π···π interactions with the centroid–centroid distance of 3.9311(13) Å.

Crystal structure of a Zn-doped derivative of the Li17Ge4 compound

International Nuclear Information System (INIS)

Lacroix-Orio, L.; Tillard, M.; Belin, C.

2008-01-01

The compound Li 17-ε Zn ε Ge 4 has been obtained as a side product during the preparation of the intermetallic compound Li 8 Zn 2 Ge 3 from the elements. Its structure has been determined from single crystal X-ray diffraction intensities measured at 173 K. It crystallizes in the cubic system, F4-bar3m space group, a = 18.842(1) A, Z = 20. Its crystal structure is slightly different from those so far reported in the literature for the Zn-free phase Li 17 Ge 4 , particularly concerned are the positions and the site occupations of Li atoms. Most likely, these structural variations result from the presence of a small Zn concentration in the compound. The Zn doping atom has been found only at the specific Li 4d site (about 3 at.% Zn)

The crystal structure of kudriavite, (Cd,Pb)Bi2S4

DEFF Research Database (Denmark)

Balic Zunic, Tonci; Makovicky, Emil

2007-01-01

The crystal structure of kudriavite, (Cd,Pb)Bi2S4, a new mineral species, was solved from single-crystal X-ray-diffraction data and refi ned to R = 4.9% (4.3% for a model with split mixed-cation sites). Lattice parameters are a 13.095(1), b 4.0032(3), c 14.711(1) Å, 115.59(1)°, V 695.6(1) Å3....... The structure is equivalent to that of synthetic CdBi2S4, space group C2/m, Z = 4, and represents a pavonite homologue, N = 3. It is built of three-octahedron-thick columns of (311)PbS-like slabs combined by "unitcell twinning" in a quasi-mirror-glide succession. The slabs, which are intrinsically of the same...... topology, differ in the coordination state of bordering cations because of the relative positions of the adjacent layers. In the slabs of type I (the "non-accreting" slab common to all pavonite homologues), the central columns of octahedra are fl anked by half-octahedral (square-pyramidal) coordinations...

SYNTHESIS, THERMAL STUDIES AND CRYSTAL STRUCTURE OF 4-AMINOPYRIDINIUM SEMI-OXALATE HEMIHYDRATE

Directory of Open Access Journals (Sweden)

CECILIA CHACÓN

2017-06-01

Full Text Available The title compound has been synthesized by grinding in an agate mortar. Its structure was characterized by TGA-DSC studies and single-crystal X-ray diffraction. This compound crystallize in the monoclinic system with space group C2/c, Z = 4, and unit cell parameters a = 16.109(2 Å, b = 5.748(7 Å, c = 20.580(3 Å, β = 107.36(1°. The salt, C2HO4-.C5H7N+.0.5 H2O, is an ionic ensemble assisted by hydrogen bonds established between 4-aminopyridinium cations, oxalate anions and water molecules. The three components thus construct a supramolecular assembly with a three-dimensional hydrogen bonded framework.

Crystal structure of 1-methyl-4-methylsulfanyl-1H-pyrazolo[3,4-d]pyrimidine

Directory of Open Access Journals (Sweden)

Mohammed El Fal

2014-12-01

Full Text Available In the title compound, C7H8N4S, the non-H atoms of the pyrazolo[3,4-d]pyrimidine ring system and the methylsulfanyl group lie on a crystallographic mirror plane. In the crystal, molecules are linked via a number of π–π interactions [centroid–centroid distances vary from 3.452 (7 to 3.6062 (8 Å], forming a three-dimensional structure.

Mechanochemical synthesis and crystal structure of a 1:2 co-crystal of 1,3,6,8-tetraazatricyclo[4.3.1.13,8]undecane (TATU and 4-chloro-3,5-dimethylphenol

Directory of Open Access Journals (Sweden)

Augusto Rivera

2016-11-01

Full Text Available Solvent-free treatment of 1,3,6,8-tetraazatricyclo[4.3.1.13,8]undecano (TATU with 4-chloro-3,5-dimethylphenol led to the formation of the title co-crystal, C7H14N4·2C8H9ClO. The asymmetric unit contains one aminal cage molecule and two phenol molecules linked via two O—H...N hydrogen bonds. In the aminal cage, the N–CH2–CH2–N unit is slightly distorted from a syn periplanar geometry. Aromatic π–π stacking between the benzene rings from two different neighbouring phenol molecules [centroid–centroid distance = 4.0570 (11 Å] consolidates the crystal packing.

Origin of electronic properties of PbGa2Se4 crystal: Experimental and theoretical investigations

International Nuclear Information System (INIS)

Babuka, T.; Kityk, I.V.; Parasyuk, O.V.; Myronchuk, G.; Khyzhun, O.Y.; Fedorchuk, A.O.; Makowska-Janusik, M.

2015-01-01

Graphical abstract: In the presented work the structural and electronic properties of the PbGa 2 Se 4 single crystal were investigated experimentally as well as theoretically. The XPS spectra, Urbach’s rule and steepness parameters of PbGa 2 Se 4 single crystal have been investigated for the first time. The quantum chemical calculations were also never performed before for the studied structure. The theoretically obtained data help to explain the properties of material. - Highlights: • Urbach’s rule and steepness parameters for PbGa 2 Se 4 crystals explored for the first time. • Non-reactivity of the PbGa 2 Se 4 surface was established by XPS. • DFT approach shows its efficiency to describe electronic properties of PbGa 2 Se 4 . • Electronic parameters are affected by existence of electron–phonon interaction. - Abstract: The PbGa 2 Se 4 crystal is a promising material for optoelectronic applications. It is caused by coexistence of the large polarized Pb cations and a huge contribution of anharmonic phonon subsystem caused by chalcogenide anions. In the present work the electronic and optical properties of the mentioned material were studied theoretically as well as experimentally by optical and X-ray photoelectron spectroscopy methods. The DFT approach has been used for the quantum chemical electronic properties calculations. Urbach rule and steepness parameters of the PbGa 2 Se 4 crystal have been evaluated for the first time. These parameters and Urbach energies increase with increasing temperature of the samples that is typical for the semiconducting materials. The XPS measurements of the investigated crystal reveal that all the spectral features are originated from core-level states of the constituent elements. Simultaneously these results also confirm non-reactivity of the PbGa 2 Se 4 surface. However, the titled single crystal possesses a number of intrinsic structural defects and vacancies thereby affecting its electronic properties. The

Sources of optical distortion in rapidly grown crystals of KH2PO4

International Nuclear Information System (INIS)

De Yoreo, J.J.; Zaitseva, N.P.; Woods, B.W.; Land, T.A.; Rek, Z.U.

1995-01-01

We report results of x-ray topographic and optical measurements on KH 2 PO 4 crystals grown at rates of 5 to 30mm/day. We show that optical distortion in these crystals is caused primarily by 3 sources: dislocations, differences in composition between adjacent growth sectors of the crystal, and differences in composition between adjacent sectors of vicinal growth hillocks within a single growth sector of the crystal. We find that the compositional heterogeneities cause spatial variations in the refractive index and induced distortion of the transmitted wave front while large groups of dislocations are responsible for strain induced birefringence which leads to beam depolarization

Crystal structure and characterization of the novel NH{sup +} Midline-Horizontal-Ellipsis N hydrogen bonded polar crystal [NH{sub 2}(CH{sub 2}){sub 4}NH][BF{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Wojtas, M., E-mail: maciej.wojtas@chem.uni.wroc.pl [Faculty of Chemistry, University of Wroclaw, Joliot-Curie 14, 50-383 Wroclaw (Poland); Gagor, A. [W. Trzebiatowski Institute of Low Temperature and Structure Research, Polish Academy of Science, PO Box 1410, 50-950 Wroclaw (Poland); Czupinski, O. [Faculty of Chemistry, University of Wroclaw, Joliot-Curie 14, 50-383 Wroclaw (Poland); Medycki, W. [Institute of Molecular Physics, Polish Academy of Science, Smoluchowskiego 17, 60-179 Poznan (Poland); Jakubas, R. [Faculty of Chemistry, University of Wroclaw, Joliot-Curie 14, 50-383 Wroclaw (Poland)

2012-03-15

Dielectric properties and phase transitions of the piperazinium tetrafluoroborate ([NH{sub 2}(CH{sub 2}){sub 4}NH][BF{sub 4}], abbreviated as PFB) crystal are related to the one-dimensional arrangement of the cations linked by the bistable NH{sup +} Midline-Horizontal-Ellipsis N hydrogen bonds and molecular motions of the [BF{sub 4}]{sup -} units. The crystal structure of [NH{sub 2}(CH{sub 2}){sub 4}NH][BF{sub 4}] is monoclinic at room temperature with the polar space group Pn. The polar/acentric properties of the room temperature phase IV have been confirmed by the piezoelectric and pyroelectric measurements. DSC measurements show that the compound undergoes three first-order structural phase transitions: at 421/411 K (heating/cooling), at 386/372 K and at 364/349 K. {sup 1}H and {sup 19}F NMR measurements indicate the reorientational motions of [BF{sub 4}]{sup -} anions and piperazinium(+) cations as well as the proton motion in the hydrogen-bonded chains of piperazine along the [001] direction. Over the phase I the isotropic reorientational motions or even self-diffusion of the cations and anions are expected. The conductivity measurements in the vicinity of the II-I PT indicate a superionic phase over the phase I. - Graphical abstract: It must be emphasized that the titled compound represents the first organic-inorganic simple salt containing the single-protonated piperazinium cation which was studied by means of the wide variety of experimental techniques. A survey of Cambridge Structural Database (CSD version 5.32 (November 2010) and updates (May 2011)) for structure containing the piperazinium cations yields 248 compounds with the doubly protonated piperazinium(2+) cations and only eight compounds with the singly protonated piperazinium(+) cations. Among these structures only one is the hybrid organic-inorganic material. This is piperazinium nitrate characterized structurally. The crystal packing of [NH{sub 2}(CH{sub 2}){sub 4}NH][BF{sub 4}], phase IV. The

of Nd3+ions in YLiF4 and LuLiF4 crystals

Directory of Open Access Journals (Sweden)

André Felipe Henriques Librantz

2006-01-01

Full Text Available Nd3+ ultraviolet (UV fluorescence induced by multiphotonic laser excitations was studied in doped Nd:YLiF4 (YLF and Nd:LuLiF4 (LLF crystals by using the time resolved spectroscopy technique. The UV luminescences are due to transitions between the 4f25d and the 4f3 electronic configurations of Nd3+ ions. The 4f25d configuration can be reached by direct pumping or by multiphotonic excitation, both processes give rise to the UV band emission with structure due to the strong phonon coupling expected for 5d orbital involvement in the transition. The multiphotonic excitation process is due to three photons (532 nanometers [nm] sequential absorptions by metastable levels of the 4f3 configuration split by crystalline local field. The sequential excitation of Nd by the laser excitation is attributed to the 4I9/2 + 532 nm t 4G7/2 ground state absorption followed by the 4G7/2 + 532 nm t 2F5/2 and 2F5/2 + 532 nm t 4f25d excited state absorptions. The UV emissions due to 4f25d configuration are parity allowed, having lifetime of 35 nanoseconds (ns in contrast to UV emissions from 4f3 configuration which are induced by two absorption steps and are parity forbidden showing longer lifetime of 8 microseconds (ms and narrow lines. The polarization effects of the UV emissions were studied and their behaviors are dependent on the excited state configuration involving or not involving the 5d orbital. The allowed UV emission positions were affected by the host variation more than the ones originated from the 4f3 configuration as expected. The electronic energy of the 4f25d configuration shifts to lower energy for increasing the crystal field.

Crystallization and preliminary X-ray analysis of eukaryotic initiation factor 4E from Pisum sativum

International Nuclear Information System (INIS)

Ashby, Jamie A.; Stevenson, Clare E. M.; Maule, Andrew J.; Lawson, David M.

2009-01-01

Crystals of N-terminally truncated eIF4E from pea were obtained and X-ray data were recorded in-house to a resolution of 2.2 Å. Crystals of an N-terminally truncated 20 kDa fragment of Pisum sativum eIF4E (ΔN-eIF4E) were grown by vapour diffusion. X-ray data were recorded to a resolution of 2.2 Å from a single crystal in-house. Indexing was consistent with primitive monoclinic symmetry and solvent-content estimations suggested that between four and nine copies of the eIF4E fragment were possible per crystallographic asymmetric unit. eIF4E is an essential component of the eukaryotic translation machinery and recent studies have shown that point mutations of plant eIF4Es can confer resistance to potyvirus infection

High-quality single crystal growth and magnetic property of Mn4Ta2O9

Science.gov (United States)

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 growth and magnetic property of a new compound CeAu4Si2

International Nuclear Information System (INIS)

Nakashima, Hiroshi; Thamizhavel, Arumugam; Matsuda, Tatsuma D.; Haga, Yoshinori; Takeuchi, Tetsuya; Sugiyama, Kiyohiro; Settai, Rikio; Onuki, Yoshichika

2006-01-01

We have succeeded in growing a new ternary Ce compound CeAu 4 Si 2 . This compound crystallizes in the tetragonal crystal structure P4-bar m2 (-bar 1-bar 1-bar 5) with lattice parameters a=4.3304 -bar A and c=27.409 -bar A. The local environment around Ce atoms is similar to that of the well-known ThCr 2 Si 2 -type tetragonal structure in CeAu 2 Si 2 . Single crystals of CeAu 4 Si 2 were grown by the flux method using an Au 4.37 Si eutectic alloy as flux. Electrical resistivity, specific heat and magnetization measurements revealed a ferromagnetic ordering at T C =5.3 -bar K with a saturation moment of 1.7-bar μ B /Ce. Anisotropic features in the magnetic susceptibility and magnetization were well explained by a crystalline electric field (CEF) model. Estimated excitation energies from the ground state doublet to two excited doublets are 284 and 340-bar K, respectively

Crystal growth and electronic structure of low-temperature phase SrMgF{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Atuchin, Victor V. [Laboratory of Optical Materials and Structures, Institute of Semiconductor Physics, SB RAS, Novosibirsk 630090 (Russian Federation); Functional Electronics Laboratory, Tomsk State University, Tomsk 634050 (Russian Federation); Laboratory of Semiconductor and Dielectric Materials, Novosibirsk State University, Novosibirsk 630090 (Russian Federation); Goloshumova, Alina A. [Laboratory of Crystal Growth, Institute of Geology and Mineralogy, SB RAS, Novosibirsk 630090 (Russian Federation); Isaenko, Ludmila I. [Laboratory of Semiconductor and Dielectric Materials, Novosibirsk State University, Novosibirsk 630090 (Russian Federation); Laboratory of Crystal Growth, Institute of Geology and Mineralogy, SB RAS, Novosibirsk 630090 (Russian Federation); Jiang, Xingxing [BCCRD, Key Laboratory of Functional Crystals and Laser Technology, Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Lobanov, Sergey I. [Laboratory of Crystal Growth, Institute of Geology and Mineralogy, SB RAS, Novosibirsk 630090 (Russian Federation); Zhang, Zhaoming [Australian Nuclear Science & Technology Organisation, Lucas Heights, NSW 2234 (Australia); Lin, Zheshuai, E-mail: zslin@mail.ipc.ac.cn [BCCRD, Key Laboratory of Functional Crystals and Laser Technology, Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190 (China)

2016-04-15

Using the vertical Bridgman method, the single crystal of low temperature phase SrMgF{sub 4} is obtained. The crystal is in a very good optical quality with the size of 10×7×5 mm{sup 3}. Detailed photoemission spectra of the element core levels are determined by a monochromatic AlKa (1486.6 eV) X-ray source. Moreover, the first-principles calculations are performed to investigate the electronic structure of SrMgF{sub 4}. A good agreement between experimental and calculated results is achieved. It is demonstrated that almost all the electronic orbitals are strongly localized and the hybridization with the others is very small, but the Mg–F bonds covalency is relatively stronger than that of Sr–F bonds. - Graphical abstract: Large size of low-temperature phase SrMgF{sub 4} crystal was obtained (right) and its electronic structure was investigated by X-ray photoelectron spectroscopy and first-principles calculation (left). - Highlights: • Large size single crystal of low-temperature phase SrMgF{sub 4} is obtained. • Electronic structure of SrMgF{sub 4} is measured by X-ray photoelectron spectroscopy. • Partial densities of states are determined by first-principles calculation. • Good agreement between experimental and calculated results is achieved. • Strong ionic characteristics of chemical bonds are exhibited in SrMgF{sub 4}.

Characterization of PbWO4 crystals for high-energy physics experiments

Science.gov (United States)

Kim, M. J.; Park, H.; Kim, H. J.

2016-09-01

High-energy physics (HEP) experiments have employed many new types of scintillators. Specifically, bismuth germanate, thallium-doped cesium iodide, and lead tungstate (PbWO4, PWO) have been used for the L3 experiment; CLEO II, Belle and BES-III; and CMS, respectively. PWO has particularly beneficial properties, such as high density, fast decay time, short radiation length and radiation hardness. In this study, we tested the PWO crystals at low temperatures to determine their applicability in future calorimeters. Various crystals from the Proton Antiproton Annihilations at Darmstadt (PANDA) experiment in Giessen, the Bogoroditsk Techno-Chemical Plant (BTCP) in Russia and by Shanghai Institute of Ceramics, Chinese Academy of Sciences (SICCAS) in China were investigated. We studied the scintillation properties of PWO crystals, such as their X-ray luminescence, relative light yields, absolute light yields, energy resolutions, decay times and longitudinal uniformities of their light yields. In addition, we measured the temperature dependences of the light yields and decay times by using a 137Cs γ-ray source. The emission spectra of the PWO crystals consisted of a broad band from 350 nm to 700 nm, and the peak emission wavelength in each spectrum was 420 nm. The emission spectra of the PWO crystals from SICCAS were slightly shifted to longer wavelengths compared with those of the crystals from the other institutions.

Crystal Structure and Spectroscopic Characterization of K8(VO)2O(SO4)6:

DEFF Research Database (Denmark)

Rasmussen, Søren Birk; Rasmussen, Rikke Christina; Fehrmann, Rasmus

2003-01-01

Red and yellow dichroistic crystals of a vanadium(V) compound, potassium (mu-oxo, di-mu-suifato)bis(oxodisulfato-vanadate), K-8(VO)(2)O(SO4)(6), have been obtained from the ternary catalytic model melt system K2S2O7-K2SO4-V2O5. By slow cooling of the melt from 420 to 355 degreesC, crystal growth...

crystal

Science.gov (United States)

Yu, Yi; Huang, Yisheng; Zhang, Lizhen; Lin, Zhoubin; Sun, Shijia; Wang, Guofu

2014-07-01

A Nd3+:Na2La4(WO4)7 crystal with dimensions of ϕ 17 × 30 mm3 was grown by the Czochralski method. The thermal expansion coefficients of Nd3+:Na2La4(WO4)7 crystal are 1.32 × 10-5 K-1 along c-axis and 1.23 × 10-5 K-1 along a-axis, respectively. The spectroscopic characteristics of Nd3+:Na2La4(WO4)7 crystal were investigated. The Judd-Ofelt theory was applied to calculate the spectral parameters. The absorption cross sections at 805 nm are 2.17 × 10-20 cm2 with a full width at half maximum (FWHM) of 15 nm for π-polarization, and 2.29 × 10-20 cm2 with a FWHM of 14 nm for σ-polarization. The emission cross sections are 3.19 × 10-20 cm2 for σ-polarization and 2.67 × 10-20 cm2 for π-polarization at 1,064 nm. The fluorescence quantum efficiency is 67 %. The quasi-cw laser of Nd3+:Na2La4(WO4)7 crystal was performed. The maximum output power is 80 mW. The slope efficiency is 7.12 %. The results suggest Nd3+:Na2La4(WO4)7 crystal as a promising laser crystal fit for laser diode pumping.

Electronic structure and pair potential energy analysis of 4-n-methoxy-4′-cyanobiphenyl: A nematic liquid crystal

Energy Technology Data Exchange (ETDEWEB)

Sharma, Dipendra, E-mail: d-11sharma@rediffmail.com; Tiwari, S. N., E-mail: sntiwari123@rediffmail.com [Department of Physics, DDU Gorakhpur University, Gorakhpur (India); Dwivedi, M. K., E-mail: dwivedi-ji@gmail.com [Department of Physics, Banaras Hindu University, Varanasi (India)

2016-05-06

Electronic structure properties of 4-n-methoxy-4′-cyanobiphenyl, a pure nematic liquid crystal have been examined using an ab‒initio, HF/6‒31G(d,p) technique with GAMESS program. Conformational and charge distribution analysis have been carried out. MEP, HOMO and LUMO surfaces have been scanned. Ionization potential, electron affinity, electronegativity, global hardness and softness of the liquid crystal molecule have been calculated. Further, stacking, side by side and end to end interactions between a molecular pair have been evaluated. Results have been used to elucidate the physico-chemical and liquid crystalline properties of the system.

Crystallization and preliminary X-ray diffraction analysis of motif N from Saccharomyces cerevisiae Dbf4

International Nuclear Information System (INIS)

Matthews, Lindsay A.; Duong, Andrew; Prasad, Ajai A.; Duncker, Bernard P.; Guarné, Alba

2009-01-01

To understand the role of the Cdc7–Dbf4 complex in checkpoint responses, a fragment of Saccharomyces cerevisiae Dbf4 encompassing motif N was isolated, overproduced and crystallized. The Cdc7–Dbf4 complex plays an instrumental role in the initiation of DNA replication and is a target of replication-checkpoint responses in Saccharomyces cerevisiae. Cdc7 is a conserved serine/threonine kinase whose activity depends on association with its regulatory subunit, Dbf4. A conserved sequence near the N-terminus of Dbf4 (motif N) is necessary for the interaction of Cdc7–Dbf4 with the checkpoint kinase Rad53. To understand the role of the Cdc7–Dbf4 complex in checkpoint responses, a fragment of Saccharomyces cerevisiae Dbf4 encompassing motif N was isolated, overproduced and crystallized. A complete native data set was collected at 100 K from crystals that diffracted X-rays to 2.75 Å resolution and structure determination is currently under way

Phase relations in Ca(Sr)MoO4-Ln2(NoO4)3 systems (Ln = Pr-Lu)

International Nuclear Information System (INIS)

Vakalyuk, V.V.; Evdokimov, A.A.; Berezina, T.A.

1982-01-01

Using the methods of X-ray phase and differential thermal analyses phase ratios in the systems Ca(Sr)MoO 4 -Ln 2 (MoO 4 ) 3 at Ln=Pr-Lu are studied and phase diagrams of the systems CaMoO 4 -Ln 2 (MoO 4 ) 3 , for Ln=Nd, Gd, Yb and SrMoO 4 -Sm 2 (MoO 4 ) 3 are built. It is shown that phase ratios in the systems are similar for the following groups of rare earths: Pr-Sm, Eu-Tb, Ho-Lu. In the first group of systems ordered phase over all subsolidus region are formed, in the second one - ordered phases with scheelite-like structure and wide regions of homogeneity on the basis of Ca(Sr)MoO 4 are formed above the temperature of polymorphous transformation of rare earth molybdates, for the third group of systems intermediate compounds are not detected

Overexpression, crystallization and preliminary X-ray crystallographic analysis of erythronate-4-phosphate dehydrogenase from Pseudomonas aeruginosa

Energy Technology Data Exchange (ETDEWEB)

Ha, Jun Yong; Lee, Ji Hyun; Kim, Kyoung Hoon; Kim, Do Jin; Lee, Hyung Ho; Kim, Hye-Kyung; Yoon, Hye-Jin; Suh, Se Won, E-mail: sewonsuh@snu.ac.kr [Department of Chemistry, College of Natural Sciences, Seoul National University, Seoul 151-742 (Korea, Republic of)

2006-02-01

Erythronate-4-phosphate dehydrogenase from P. aeruginosa was crystallized and X-ray diffraction data were collected to 2.20 Å resolution. 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 B{sub 6} (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 P2{sub 1}2{sub 1}2{sub 1}, 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{sub M}) of 3.64 Å{sup 3} Da{sup −1} and a solvent content of 66%.

Overexpression, crystallization and preliminary X-ray crystallographic analysis of erythronate-4-phosphate dehydrogenase from Pseudomonas aeruginosa

International Nuclear Information System (INIS)

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

Erythronate-4-phosphate dehydrogenase from P. aeruginosa was crystallized and X-ray diffraction data were collected to 2.20 Å resolution. 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 B 6 (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 P2 1 2 1 2 1 , 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 Å 3 Da −1 and a solvent content of 66%

Crystal structure and energy band and optical properties of phosphate Sr3P4O13

International Nuclear Information System (INIS)

Zhang, Y.-C.; Cheng, W.-D.; Wu, D.-S.; Zhang, H.; Chen, D.-G.; Gong, Y.-J.; Kan, Z.-G.

2004-01-01

A single crystal of the compound Sr 3 P 4 O 13 has been found and the crystal structure has been characterized by means of single crystal X-ray diffraction analysis. The compound crystallizes in triclinic system and belongs to space group P1-bar. It builds up from SrO 7 polyhedra and P 4 O 13 -6 anions and has a layered structure, and the Sr atoms are located in the interlayer space. The absorption and luminescence spectrum of Sr 3 P 4 O 13 microcrystals have been measured. The calculated results of crystal energy band structure by the DFT show that the solid state of Sr 3 P 4 O 13 is an isolator with direct band gap. The calculated total and partial density of states indicate that the top valence bands are contributions from P 3p and O 2p states and low conduction bands mostly originate from Sr atomic states. The calculated optical response functions expect that the Sr 3 P 4 O 13 is a low refractive index, and it is possible that the Sr 3 P 4 O 13 is used to make transparent material between the UV and FR light zone

Optical energy gaps and photoluminescence peaks of BaGa2S4:Er3+ and BaGa2Se4:Er3+ single crystals

International Nuclear Information System (INIS)

Choe, Sung-Hyu; Jin, Moon-Seog; Kim, Wha-Tek

2005-01-01

BaGa 2 S 4 :Er 3+ and BaGa 2 Se 4 :Er 3+ single crystals were grown by using the chemical transport reaction method. The optical energy gaps of the BaGa 2 S 4 :Er 3+ and the BaGa 2 Se 4 :Er 3+ single crystals were found to be 4.045 eV and 3.073 eV, respectively, at 11 K. The temperature dependence of the optical energy gap was well fitted by the Varshni equation. Sharp emission peaks were observed in the photoluminescence spectra of the single crystals and assigned to radiation recombination between split Stark levels of the Er 3+ ion.

Crystal structures of three co-crystals of 1,2-bis-(pyridin-4-yl)ethane with 4-alk-oxy-benzoic acids: 4-eth-oxy-benzoic acid-1,2-bis-(pyridin-4-yl)ethane (2/1), 4-n-propoxybenzoic acid-1,2-bis(pyridin-4-yl)ethane (2/1) and 4-n-but-oxy-benzoic acid-1,2-bis-(pyridin-4-yl)ethane (2/1).

Science.gov (United States)

Tabuchi, Yohei; Gotoh, Kazuma; Ishida, Hiroyuki

2015-11-01

The crystal structures of three hydrogen-bonded co-crystals of 4-alk-oxy-benzoic acid-1,2-bis-(pyridin-4-yl)ethane (2/1), namely, 2C9H10O3·C12H12N2, (I), 2C10H12O3·C12H12N2, (II), and 2C11H14O3·C12H12N2, (III), have been determined at 93, 290 and 93 K, respectively. In (I), the asymmetric unit consists of one 4-eth-oxy-benzoic acid mol-ecule and one half-mol-ecule of 1,2-bis-(pyridin-4-yl)ethane, which lies on an inversion centre. In (II) and (III), the asymmetric units each comprise two crystallographically independent 4-alk-oxy-benzoic acid mol-ecules and one 1,2-bis-(pyridin-4-yl)ethane mol-ecule. In each crystal, the two components are linked by O-H⋯N hydrogen bonds, forming a linear hydrogen-bonded 2:1unit of the acid and the base. Similar to the structure of 2:1 unit of (I), the units of (II) and (III) adopt nearly pseudo-inversion symmetry. The 2:1 units of (I), (II) and (III) are linked via C-H⋯O hydrogen bonds, forming tape structures.

Thermal, spectral and laser characteristics of Nd doped La0.05Lu0.95VO4 crystal

Science.gov (United States)

Xu, Honghao; Han, Shuo; Yu, Haohai; Wang, Zhengping; Wang, Jiyang; Zhang, Huaijin; Tang, Dingyuan

2014-02-01

A 0.25 at% Nd doped La0.05Lu0.95VO4 mixed crystal was grown by the Czochralski method. The thermal properties including thermal expansion, specific heat, thermal diffusion, and thermal conductivity were systematically studied. Meanwhile the reasons for cracking of this mixed crystal were also discussed. The refractive index at wavelengths of 633 nm and 1539 nm were obtained with the prism coupling method. The polarized absorption and fluorescence spectra of the crystal were also measured at room temperature. It was found that the fluorescence lifetime of 4F3/2 manifold for Nd3+ in Nd:La0.05Lu0.95VO4 is about 90 μs. Diode-pumped continuous-wave (CW) laser operations at 1.06 μm with a- and c-cut crystals were demonstrated. For the a-cut crystal a maximum output power of 5.41 W was obtained at an incident pump power of 12.9 W. Different from the a-cut crystal, the laser spectrum of the c-cut crystal was found to be dual-wavelength.

A new crystal modification of diammonium hydrogen phosphate, (NH42(HPO4

Directory of Open Access Journals (Sweden)

Bernhard Spingler

2010-04-01

Full Text Available The addition of hexafluoridophosphate salts (ammonium, silver, thallium or potassium is usually used to precipitate complex cations from aqueous solutions. It has long been known that PF6− is sensitive towards hydrolysis under acidic conditions [Gebala & Jones (1969. J. Inorg. Nucl. Chem. 31, 771–776; Plakhotnyk et al. (2005. J. Fluorine Chem. 126, 27–31]. During the course of our investigation into coinage metal complexes of diphosphine ligands, we used ammonium hexafluoridophosphate in order to crystallize [Ag(diphosphine2]PF6 complexes. From these solutions we always obtained needle-like crystals which turned out to be the title compound, 2NH4+·HPO42−. It was received as the hydrolysis product of NH4PF6. The crystals are a new modification of diammonium hydrogen phosphate. In contrast to the previously published polymorph [Khan et al. (1972. Acta Cryst. B28, 2065–2069], Z′ of the title compound is 2. In the new modification of the title compound, there are eight molecules of (NH42(HPO4 in the unit cell. The structure consists of PO3OH and NH4 tetrahedra, held together by O—H...O and N—H...O hydrogen bonds.

Non linear optical studies on semiorganic single crystal: L-arginine 4-nitrophenalate 4-nitrophenol dihydrate (LAPP)

Science.gov (United States)

Mahadevan, M.; Sankar, P. K.; Vinitha, G.; Arivanandhan, M.; Ramachandran, K.; Anandan, P.

2017-07-01

L-arginine 4-nitrophenalate 4-nitrophenol dihydrate (LAPP) has been synthesized and grown by solution growth at room temperature using deionized water as a solvent. The various functional groups of the sample were identified by Fourier transform infra-red and Fourier transforms - Raman spectroscopic analyses. The Laser damage threshold of LAPP has been studied. Refractive index of LAPP single crystal was measured using Metricon prism coupler Instrument. The etching studies were carried out to study the quality of the grown crystals. The third order nonlinear optical properties of LAPP sample was analyzed by the Z-scan technique using 532 nm diode pumped CW Nd: YAG laser. The LAPP material exhibits negative optical nonlinearity. The results show that LAPP sample has potential applications in nonlinear optics and it can be exploited for optical limiting or switching.

Radiation hardness qualification of PbWO4 scintillation crystals for the CMS Electromagnetic Calorimeter

CERN Document Server

Adzic, P.; Andelin, D.; Anicin, I.; Antunovic, Z.; Arcidiacono, R.; Arenton, M.W.; Auffray, E.; Argiro, S.; Askew, A.; Baccaro, S.; Baffioni, S.; Balazs, M.; Bandurin, D.; Barney, D.; Barone, L.M.; Bartoloni, A.; Baty, C.; Beauceron, S.; Bell, K.W.; Bernet, C.; Besancon, M.; Betev, B.; Beuselinck, R.; Biino, C.; Blaha, J.; Bloch, P.; Borisevitch, A.; Bornheim, A.; Bourotte, J.; Brown, R.M.; Buehler, M.; Busson, P.; Camanzi, B.; Camporesi, T.; Cartiglia, N.; Cavallari, F.; Cecilia, A.; Chang, P.; Chang, Y.H.; Charlot, C.; Chen, E.A.; Chen, W.T.; Chen, Z.; Chipaux, R.; Choudhary, B.C.; Choudhury, R.K.; Cockerill, D.J.A.; Conetti, S.; Cooper, S.I.; Cossutti, F.; Cox, B.; Cussans, D.G.; Dafinei, I.; Da Silva Di Calafiori, D.R.; Daskalakis, G.; David, A.; Deiters, K.; Dejardin, M.; De Benedetti, A.; Della Ricca, G.; Del Re, D.; Denegri, D.; Depasse, P.; Descamps, J.; Diemoz, M.; Di Marco, E.; Dissertori, G.; Dittmar, M.; Djambazov, L.; Djordjevic, M.; Dobrzynski, L.; Dolgopolov, A.; Drndarevic, S.; Drobychev, G.; Dutta, D.; Dzelalija, M.; Elliott-Peisert, A.; El Mamouni, H.; Evangelou, I.; Fabbro, B.; Faure, J.L.; Fay, J.; Fedorov, A.; Ferri, F.; Franci, D.; Franzoni, G.; Freudenreich, K.; Funk, W.; Ganjour, S.; Gascon, S.; Gataullin, M.; Gentit, F.X.; Ghezzi, A.; Givernaud, A.; Gninenko, S.; Go, A.; Gobbo, B.; Godinovic, N.; Golubev, N.; Govoni, P.; Grant, N.; Gras, P.; Haguenauer, M.; Hamel de Monchenault, G.; Hansen, M.; Haupt, J.; Heath, H.F.; Heltsley, B.; Cornell U., LNS.; Hintz, W.; Hirosky, R.; Hobson, P.R.; Honma, A.; Hou, G.W.S.; Hsiung, Y.; Huhtinen, M.; Ille, B.; Ingram, Q.; Inyakin, A.; Jarry, P.; Jessop, C.; Jovanovic, D.; Kaadze, K.; Kachanov, V.; Kailas, S.; Kataria, S.K.; Kennedy, B.W.; Kokkas, P.; Kolberg, T.; Korjik, M.; Krasnikov, N.; Krpic, D.; Kubota, Y.; Kuo, C.M.; Kyberd, P.; Kyriakis, A.; Lebeau, M.; Lecomte, P.; Lecoq, P.; Ledovskoy, A.; Lethuillier, M.; Lin, S.W.; Lin, W.; Litvine, V.; Locci, E.; Longo, E.; Loukas, D.; Luckey, P.D.; Lustermann, W.; Ma, Y.; Malberti, M.; Malcles, J.; Maletic, D.; Manthos, N.; Maravin, Y.; Marchica, C.; Marinelli, N.; Markou, A.; Markou, C.; Marone, M.; Matveev, V.; Mavrommatis, C.; Meridiani, P.; Milenovic, P.; Mine, P.; Missevitch, O.; Mohanty, A.K.; Moortgat, F.; Musella, P.; Musienko, Y.; Nardulli, A.; Nash, J.; Nedelec, P.; Negri, P.; Newman, H.B.; Nikitenko, A.; Nessi-Tedaldi, F.; Obertino, M.M.; Organtini, G.; Orimoto, T.; Paganoni, M.; Paganini, P.; Palma, A.; Pant, L.; Papadakis, A.; Papadakis, I.; Papadopoulos, I.; Paramatti, R.; Parracho, P.; Pastrone, N.; Patterson, J.R.; Pauss, F.; Peigneux, J.P.; Petrakou, E.; Phillips, D.G.; Piroue, P.; Ptochos, F.; Puljak, I.; Pullia, A.; Punz, T.; Puzovic, J.; Ragazzi, S.; Rahatlou, S.; Rander, J.; Razis, P.A.; Redaelli, N.; Renker, D.; Reucroft, S.; Ribeiro, P.; Rogan, C.; Ronquest, M.; Rosowsky, A.; Rovelli, C.; Rumerio, P.; Rusack, R.; Rusakov, S.V.; Ryan, M.J.; Sala, L.; Salerno, R.; Schneegans, M.; Seez, C.; Sharp, P.; Shepherd-Themistocleous, C.H.; Shiu, J.G.; Shivpuri, R.K.; Shukla, P.; Siamitros, C.; Sillou, D.; Silva, J.; Silva, P.; Singovsky, A.; Sirois, Y.; Sirunyan, A.; Smith, V.J.; Stockli, F.; Swain, J.; Tabarelli de Fatis, T.; Takahashi, M.; Tancini, V.; Teller, O.; Theofilatos, K.; Thiebaux, C.; Timciuc, V.; Timlin, C.; Titov, Maxim P.; Topkar, A.; Triantis, F.A.; Troshin, S.; Tyurin, N.; Ueno, K.; Uzunian, A.; Varela, J.; Verrecchia, P.; Veverka, J.; Virdee, T.; Wang, M.; Wardrope, D.; Weber, M.; Weng, J.; Williams, J.H.; Yang, Y.; Yaselli, I.; Yohay, R.; Zabi, A.; Zelepoukine, S.; Zhang, J.; Zhang, L.Y.; Zhu, K.; Zhu, R.Y.

2010-01-01

Ensuring the radiation hardness of PbWO4 crystals was one of the main priorities during the construction of the electromagnetic calorimeter of the CMS experiment at CERN. The production on an industrial scale of radiation hard crystals and their certification over a period of several years represented a difficult challenge both for CMS and for the crystal suppliers. The present article reviews the related scientific and technological problems encountered.

Utilization of Snail (Achatina fulica Shell Waste for Synthesis of Calcium Tartrate Tetrahydrate (CaC4H4O6.4H2O Single Crystals in Silica Gel

Directory of Open Access Journals (Sweden)

Imam Sakdi

2012-01-01

Full Text Available Snail (Achatina fulica shell waste is massively produced by many home industries in Indonesia, especially in East Java. The snail shell is known for high calcium; therefore it is potential to be used as calcium source of supernatant in the synthesis of piezoeletric material, such as single crystal of calcium tartrate tetrahydrate (CaTT. The aim of this research is to study the synthesis and characterization of CaTT or CaC4H4O6.4H2O from snail shell waste in silica gel. Supernatant solution of CaCl2 was prepared from CaO, which previously made by calcinating the shell at 1000°C, and then reacted with HCl 1,5M. Synthesis of CaTT was conducted in a single-tube reaction at room temperature in which silica gel was used as growth medium with gelling time of 10 days and growth time of 2 weeks. The pH of gel and CaCl2 concentration were varied, 3.00; 3.50; 4.00; 4.50; 5.00; and 0.27; 0.36; 0.45; 0.54 M respectively, in order to obtain optimum condition of the synthesis, which is indicated from crystal yields. The synthesized crystals were characterized by atomic adsorption spectrophotometry (AAS, infrared spectroscopy (IR and powder X-ray diffraction (XRD. Experimental data shows that optimum condition was obtained at pH of 3.50 and [CaCl2] of 0.45M with yield of 69.37%. The obtained single crystal has clear color and octahedral-like shape with size ranged between 4 – 9 mm. Analysis data by FTIR and powder XRD confirmed that the obtained crystal was CaTT single crystals with crystal system of orthorhombic.

Growth of ZrSiO4 single crystal by flux method

International Nuclear Information System (INIS)

Ushio, Masumi; Nishitani, Yoshinari

1982-01-01

ZrSiO 4 single crystals were grown from the Na 2 O.3 V 2 O 5 fluxed melt at constant soaking temperatures of 900 0 C and 1000 0 C for periods up to 1710h, using the natural zircon seeds. Temperature difference between the seed and nutrient was 0.5 -- 5 0 C. A solubility curve of the natural zircon in Na 2 O.3 V 2 O 5 was determined. It was found that about 5.7g of the natural crystal dissolved in Na 2 O.3 V 2 O 5 in 48h at 1000 0 C and about 7.5g at 1200 0 C. .the maximum growth weight was about 0.35 2 g under conditions of the temperature difference of 2 0 C and the soaking for 1205h at 1000 0 C. The grown crystal was initially bounded with the c-, m-, p-, a-planes and very small planes consisting of the u- and x-, and finally bounded with the m- and p-planes. The observed linear growth rates of planes of ZrSiO 4 single crystals were in the following order:a(100) > c(001) > p(111) > m(110). The growth rates of a- and m-planes were about 5 -- 7 x 10 -4 mm/h and 0.9 -- 1.0 x 10 -4 mm/h, respectively. The growth hillocks of rounded triangular shape and elliptic shape extended to the direction of c-axis, were observed on the p- and m-planes, respectively. The observed step distence of the spiral and the step height were about 0.97 5 μm and 0.17 2 μm, respectively. The observed linear rate of advance of the step on the m-plane was about 0.4 0 -- 1.2 x 10 -8 cm/s. A linear growth rate of the m-plane was then calculated to be 0.2 5 -- 0.7 1 x 10 -4 mm/h by the BCF theory, which agreed in order of magnitude with the observes growth rate of the m-plabe. (author)

Recent developments in crystal calorimeters (featuring the CMS PbWO4 electromagnetic calorimeter)

International Nuclear Information System (INIS)

Gascon-Shotkin, S.

2003-01-01

In the mass range of 110-150 GeV the favored process for Higgs boson detection via p-p collisions is via its decay into two photons, which demands a very high-resolution electromagnetic calorimeter. This physics goal plus the Large Hadron Calorimeter (LHC)-imposed design constraints of 25ns bunch spacing and a hostile radiation environment have led the Compact Muon Solenoid (CMS) collaboration to the choice of lead tungstate (PbWO 4 ) crystals. These factors plus the presence of a 4T magnetic field and the relatively low room-temperature scintillation photon yield of PbWO 4 make photo detection a real challenge, which CMS has met via the choice of devices providing gain amplification: Avalanche photodiodes (APD) in the central barrel region and vacuum phototriodes (VPT) in the forward and backward endcap regions. In the past year the CMS electromagnetic calorimeter has entered the construction phase. We review progress in the areas of crystals, barrel and endcap photo detection devices, plans for detector calibration as well as the status of assembly and quality control. We also invoke relevant developments in other crystal calorimeters currently in operation or under development. Crystal calorimeters remain the medium of choice for precision energy and position measurements in high energy physics

Radiation-induced color centers in La-doped PbWO sub 4 crystals

CERN Document Server

Deng, Q; Zhu, R Y

1999-01-01

This report presents the result of a study on radiation-induced color center densities in La-doped lead tungstate (PbWO sub 4) crystals. The creation and annihilation constants of radiation-induced color centers were determined by using transmittance data measured for a PbWO sub 4 sample before and during sup 6 sup 0 Co gamma-ray irradiation at a dose rate of 15 rad/h. Following a model of color center kinetics, these constants were used to calculate color center densities under irradiations at 100 rad/h. The result was found to be in good agreement with experimental data, indicating that the behaviour of PbWO sub 4 crystals under irradiation can be predicted according to this model.

Synthesis and crystal structure of 4-(2-ammonioethylmorpholin-4-ium dichloridodiiodidocadmate/chloridotriiodidocadmate (0.90/0.10

Directory of Open Access Journals (Sweden)

Najla Mahbouli Rhouma

2016-10-01

Full Text Available The crystal structure of the title compound, (C6H16N2O[CdCl1.90I2.10], a new organic–inorganic hybrid salt synthesized in the form of single crystals, consists of discrete statistically distributed dichloridodiiodidocadmate/chloridotriiodidocadmate anions (occupancy ratio 0.90:0.10 and 4-(2-ammonioethylmorpholin-4-ium cations, [NH3(CH22NH(CH24O]2+. The cations are linked by intermolecular N—H...O hydrogen bonds, forming corrugated chains extending parallel to the c axis. The [CdCl1.90I2.10]2− tetrahalidocadmate anions lie between the chains to maximize the electrostatic interactions and are connected with the organic cations via N—H...Cl and C—H...Cl(I hydrogen bonds developing in the ab plane and leading to the formation of a three-dimensional network structure. The tetracoordinate CdII atom has a distorted tetrahedral conformation, with a τ4 index of 0.87.

Synthesis and crystal structure of lithium beryllium deuteride Li2BeD4.

Science.gov (United States)

Bulychev, Boris M; Shpanchenko, Roman V; Antipov, Evgeny V; Sheptyakov, Denis V; Bushmeleva, Svetlana N; Balagurov, Anatoly M

2004-10-04

Single-phase ternary deuteride Li(2)BeD(4) was synthesized by a high-pressure high-temperature technique from LiD and BeD(2). The crystal structure of Li(2)BeD(4) was solved from X-ray and neutron powder diffraction data. The compound crystallizes in the monoclinic space group P2(1)/c with lattice parameters a = 7.06228(9) A, b = 8.3378(1) A, c = 8.3465(1) A, beta =93.577(1) degrees, and Z = 8. Its structure contains isolated BeD(4) tetrahedra and Li atoms that are located in the structure interstices. Li(2)BeD(4) does not undergo any structural phase transitions at temperatures down to 8 K.

Synchrotron white beam topography studies of SrLaGaO4 crystals

International Nuclear Information System (INIS)

Wieteska, K.; Wierzchowski, W.; Graeff, W.; Lefeld-Sosnowska, M.; Pajaczkowska, A.; Wierzbicka, E.; Malinowska, A.

2005-01-01

Strontium lantanum gallate SrLaGaO 4 tetragonal single crystal was investigated by white beam synchrotron radiation topography. Projection and section topographs were taken in back reflection and transmission geometry. The central 'core' crystal region was practically free of defects; only one extended 'oval' defect with strong boundary contrast was observed. The strong white-black contrasts connected with elongated volume defects and cracks were observed in surrounding the 'core' region

Synthesis, crystal structure and DFT studies of N-(4-acetyl-5,5-dimethyl-4,5-dihydro-1,3,4-thiadiazol-2-yl)acetamide

Science.gov (United States)

Gautam, P.; Gautam, D.; Chaudhary, R. P.

2013-12-01

The title compound N-(4-acetyl-5,5-dimethyl-4,5-dihydro-1,3,4-thiadiazol-2-yl)acetamide ( III) was obtained from the reaction of 2-(propan-2-ylidene)hydrazinecarbothioamide ( II) with acetic anhydride instead of formation of the desired thiosemcarbazide derivative of Meldrum acid. The structures of II and III were established by elemental analysis, IR, NMR, Mass and X-ray crystallographic studies. II crystallizes in triclinic system, sp. gr. Z = 2; III crystallizes in the monoclinic system, sp. gr. P21/ c, Z = 8. Density functional theory (DFT) calculations have been carried out for III. 1H and 13C NMR of III has been calculated and correlated with experimental results.

Synthesis, crystal structure and DFT studies of N-(4-acetyl-5,5-dimethyl-4,5-dihydro-1,3,4-thiadiazol-2-yl)acetamide

International Nuclear Information System (INIS)

Gautam, P.; Gautam, D.; Chaudhary, R. P.

2013-01-01

The title compound N-(4-acetyl-5,5-dimethyl-4,5-dihydro-1,3,4-thiadiazol-2-yl)acetamide (III) was obtained from the reaction of 2-(propan-2-ylidene)hydrazinecarbothioamide (II) with acetic anhydride instead of formation of the desired thiosemcarbazide derivative of Meldrum acid. The structures of II and III were established by elemental analysis, IR, NMR, Mass and X-ray crystallographic studies. II crystallizes in triclinic system, sp. gr. P-bar1 Z = 2; III crystallizes in the monoclinic system, sp. gr. P2 1 /c, Z = 8. Density functional theory (DFT) calculations have been carried out for III. 1 H and 13 C NMR of III has been calculated and correlated with experimental results

Thermoluminescence mechanisms in CaSO4:Dy single crystals

International Nuclear Information System (INIS)

Morgan, M.D.; Stoebe, T.G.

1986-01-01

ESR studies of gamma-irradiated CaSO 4 :Dy have shown, in addition to the usual intrinsic defects, four new paramagnetic centres. An analysis of the g values and the g tensors in conjunction with the anhydrite crystal structure indicate that these centres are related to sulphate ions. Two of these centres (denoted 1a and 3a) are proposed as holes trapped and shared between two adjacent sulphate ions, this structure being stabilised by a neighbouring Ca vacancy. Centre 3b is suggested as a hole associated with one sulphate ion, again stabilised by an adjacent Ca vacancy. Because of the two distinct crystallographic directions in the anhydrite structure, centre 3b was found to consist of two distinguishable defects with slightly differing decay temperatures. The fourth centre appears to be an electron trapping site with structure similar to centre 3b. Decay temperatures of these ESR defects are correlated with the observance of TL peaks in CaSO 4 :Dy. Thermoluminescence studies as a function of impurity content confirmed the presence of calcium vacancies, which are formed during crystal growth, and that they play an important role in the TL process. TL models are proposed to account for the observed properties of CaSO 4 :Dy. (author)

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

Science.gov (United States)

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.

Crystal structure of the new ternary thorium indide Th{sub 4}Pd{sub 10}In{sub 21}

Energy Technology Data Exchange (ETDEWEB)

Hlukhyy, V.; Zaremba, V.; Stepien-Damm, J.; Troc, R

2003-03-24

The structure of Th{sub 4}Pd{sub 10}In{sub 21} was refined from single crystal X-ray diffraction data. The compound crystallizes in the monoclinic system, space group C2/m, mC70; with lattice parameters a=23.024(5) A, b=4.512(1) A, c=17.224(3) A, {beta}=124.57(3) deg. The crystal structure was refined using the SHELXL-97 program (R{sub 1}=0.0477, 2561 F{sup 2} values for 108 variables). This compound adopts the Ho{sub 4}Ni{sub 10}Ga{sub 21}-type structure. The crystal chemistry and relationships of this phase to other ones are briefly discussed.

Chemical purification of CaCO{sub 3} and CaWO{sub 4} powders used for CaWO{sub 4} crystal production for the CRESST experiment

Energy Technology Data Exchange (ETDEWEB)

Trinh Thi, H.H.; Defay, X.; Erb, A.; Hampf, R.; Lanfranchi, J.C.; Langenkaemper, A.; Morgalyuk, V.; Muenster, A.; Mondragon, E.; Oppenheimer, C.; Potzel, W.; Schoenert, S.; Steiger, H.; Ulrich, A.; Wawoczny, S.; Willers, M.; Zoeller, A. [Physik-Department and Excellence Cluster Universe, Technische Universitaet Muenchen, Garching (Germany)

2016-07-01

CRESST (Cryogenic Rare Event Search with Superconducting Thermometers) uses CaWO{sub 4} single crystals as targets for the direct search for dark matter particles. Since several years these CaWO{sub 4} crystals are grown at the Technische Universitaet Muenchen. Thereby, commercially available CaCO{sub 3} and WO{sub 3} powders are used for the synthesis of CaWO{sub 4} powder. For the experiment low intrinsic contaminations of the crystals play a crucial role. In order to improve the radiopurity of the crystals it is necessary to reduce potential sources for radioactive backgrounds such as U and Th. In this poster we will present our studies of the chemical purification of the CaCO{sub 3} and CaWO{sub 4} powders.

Crystal structure and properties of tetragonal EuAg4In8 grown by metal flux technique

International Nuclear Information System (INIS)

Subbarao, Udumula; Sarkar, Sumanta; Peter, Sebastian C.

2015-01-01

The compound EuAg 4 In 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 4 In 8 crystallizes in the CeMn 4 Al 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 4 In 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 4 In 8 was measured in the temperature range 2–300 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 4 In 8 is metallic in nature with a probable Fermi liquid behavior at low temperature. - Graphical abstract: The tetragonal EuAg 4 In 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 4 In 8 phase having tetragonal phase is grown by metal flux technique. • Magnetic and XANES measurements exhibit divalent nature of Eu in EuAg 4 In 8 . • Resistivity measurement suggests metallic nature and probable Fermi liquid behavior

Crystal structure of zdenekite NaPbCu5(AsO4)4Cl · 5H2O

International Nuclear Information System (INIS)

Zubkova, N.V.; Pushcharovsky, D.Yu.; Sarp, H.; Teat, S. J.; MacLean, E. J.

2003-01-01

The crystal structure of the mineral zdenekite NaPbCu 5 (AsO 4 ) 4 Cl · 5H 2 O was established (Bruker SMART CCD diffractometer, synchrotron radiation, λ = 0.6843 A, R = 0.096 for 1356 reflections). Single-crystal X-ray diffraction study demonstrated that zdenekite belongs to the monoclinic system with the unit-cell parameters a = 10.023(7) A, b 19.55(1) A, c = 10.023(6) A, β = 90.02(1) deg., sp. gr. P2 1 /n, Z = 4. The structure consists of polyhedral layers parallel to the (010) plane. These layers are formed by Cuφ 5 polyhedra (φ = O, Cl, H 2 O) and AsO 4 tetrahedra. Distorted Na octahedra and Pb 7-vertex polyhedra and H 2 O molecules coordinated to these metal atoms are located between the layers

Growth and optical properties of Tm:GdVO{sub 4} single crystal

Energy Technology Data Exchange (ETDEWEB)

Urata, Y.; Akagawa, K.; Wada, S.; Tashiro, H. [Photodynamics Research Center, Sendai (Japan). Inst. of Physical and Chemical Research; Suh, S.J.; Yoon, D.H. [Photodynamics Research Center, Sendai (Japan). Inst. of Physical and Chemical Research]|[Dept. of Metallurgical Engineering, Sung Kyun Kwan Univ. (Korea, Republic of); Fukuda, T. [Photodynamics Research Center, Sendai (Japan). Inst. of Physical and Chemical Research]|[Inst. for Materials Research, Tohoku Univ. (Japan)

1999-04-01

Thulium-doped gadolinium vanadate (Tm:GdVO{sub 4}) single crystal has been successfully grown by a modified Czochralski (CZ) technique. Effective distribution coefficient of Tm was determined to be 0.74. Absorption characterization was performed in the 800 nm region and the maximum absorption peak was found at 799 nm for {pi} polarization. Fluorescence spectra for tuning at the maximum absorption were obtained around 1.8-2.0 {mu}m region with 100 nm bandwidth. This suggests that a Tm:GdVO{sub 4} crystal is expected as a new promising LD pumped solid-state laser in the 2 {mu}m region. (orig.) 9 refs.

Mapping residual stresses in PbWO4 crystals using photo-elastic analysis

International Nuclear Information System (INIS)

Lebeau, M.; Gobbi, L.; Majni, G.; Paone, N.; Pietroni, P.; Rinaldi, D.

2005-01-01

Large scintillating crystals are affected by internal stresses induced by the crystal growth temperature gradient remanence. Cutting boules (ingots) into finished crystal shapes allows for a partial tension relaxation but residual stresses remain the main cause of breaking. Quality control of residual stresses is essential in the application of Scintillating Crystals to high-energy physics calorimeters (e.g. CMS ECAL at CERN LHC). In this context the industrial process optimisation towards stress reduction is mandatory. We propose a fast technique for testing samples during the production process in order to evaluate the residual stress distribution after the first phases of mechanical processing. We mapped the stress distribution in PbWO 4 slabs cut from the same production boule. The analysis technique is based on the stress intensity determination using the photo-elastic properties of the samples. The stress distribution is mapped in each sample. The analysis shows that there are regions of high residual tension close to the seed position and at the boule periphery. These results should allow for adapting the industrial process to producing crystals with lower residual stresses

Growth, spectral, dielectric and antimicrobial studies on 4-piperidinium carboxylamide picrate crystals

Science.gov (United States)

Dhanabal, T.; Tharanitharan, V.; Amirthaganesan, G.; Dhandapani, M.

2014-07-01

Single crystal of 4-piperidinium carboxylamide picrate was grown by slow evaporation solution growth technique at ambient temperature. The average dimensions of grown crystal were 0.7 × 0.3 × 0.2 cm3. The solubility of the compound was analyzed using methanol and acetone. Optical property of the compound was ascertained by UV-visible absorption spectral study. The sharp and well defined Bragg peaks observed in the powder X-ray diffraction pattern confirm its crystallinity. The different kinds of protons and carbons in the compound were confirmed by 1H and 13C NMR spectral analyses. The presence of various functional groups in the compound was assigned through polarized Raman spectral study. The mechanical property of the crystal was measured by Vicker's microhardness test and the compound was found to be soft material. The dielectric constant and dielectric loss of the crystal decrease with increase in frequency. The antibacterial and antifungal activities of the crystal were studied by disc diffusion method and found that the compound shows good inhibition efficiency against various bacteria and fungi species.

Crystal structure of CdSO4(H2O: a redetermination

Directory of Open Access Journals (Sweden)

Chatphorn Theppitak

2015-10-01

Full Text Available The crystal structure of the title compound, cadmium sulfate monohydrate or poly[(μ2-aqua(μ4-sulfatocadmium], was redetermined based on modern CMOS (complementary metal oxide silicon data. In comparison with the previous study [Bregeault & Herpin (1970. Bull. Soc. Fr. Mineral. Cristallogr. 93, 37–42], all non-H atoms were refined with anisotropic displacement parameters and the hydrogen-bonding pattern unambiguously established due to location of the hydrogen atoms. In addition, a significant improvement in terms of precision and accuracy was achieved. In the crystal, the Cd2+ cation is coordinated by four O atoms of four sulfate anions and two O atoms of water molecules, forming a distorted octahedral trans-[CdO6] polyhedron. Each sulfate anion bridges four Cd2+ cations and each water molecule bridges two Cd2+ cations, leading to the formation of a three-dimensional framework, with Cd...Cd separations in the range 4.0757 (2–6.4462 (3 Å. O—H...O hydrogen-bonding interactions of medium strength between the coordinating water molecules and sulfate anions consolidate the crystal packing.

Controlled synthesis of SrCrO4 crystals with different morphologies

International Nuclear Information System (INIS)

Yang, Xiao-Hong; Wu, Qing-Sheng; Liu, Jin-Ku

2007-01-01

Rod-shape, branch-shape, bouquet-shape and claw-shape SrCrO 4 crystals were synthesized through biomembrane/organic-addition supramolecular templates. The shapes are mainly changed with variance of the organic reagents and organic membranes. Most of the morphologies haven't been reported in the literature. This method may meet with the requirements to synthesize materials of various morphologies and size by using different supramolecular templates. This paper discusses how to control crystals' growth by supramolecular templates. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Crystal structure of 1-[2-(4-chlorophenyl-4,5-diphenyl-1H-imidazol-1-yl]propan-2-ol

Directory of Open Access Journals (Sweden)

Shaaban K. Mohamed

2017-01-01

Full Text Available The title compound, C24H21ClN2O, crystallizes with two unique molecules in the asymmetric unit. In each molecule, the central imidazole ring is substituted at the 2-, 4- and 5-positions by benzene rings. The 2-substituted ring carries a Cl atom at the 4-position. One of the imidazole N atoms in each molecule has a propan-2-ol substituent. In the crystal, a series of O—H...N, C—H...O and C—H...Cl hydrogen bonds, augmented by several C—H...π(ring interactions, generate a three-dimensional network of molecules stacked along the a-axis direction.

Crystallization and preliminary X-ray diffraction analysis of the MIF4G domain of DAP5

International Nuclear Information System (INIS)

Frank, Filipp; Virgili, Geneviève; Sonenberg, Nahum; Nagar, Bhushan

2009-01-01

The MIF4G domain of DAP5 was crystallized in two distinct crystal forms. Diffraction patterns have been analyzed and preliminary analysis, including molecular replacement, is presented here. Death-associated protein 5 (DAP5) is a member of the eIF4G family of scaffolding proteins that mediate cap-independent translation initiation by recruiting the translational machinery to internal ribosomal entry sites (IRESs) on mRNA. The MIF4G domain of DAP5 directly interacts with the eukaryotic initiation factors eIF4A and eIF3 and enhances the translation of several viral and cellular IRESs. Here, the crystallization and preliminary X-ray diffraction analysis of the MIF4G domain of DAP5 is presented

Absorption spectra of CsNd(MoO4)2 and CsGd(MoO4)2-Nd3+ crystals in strong magnetic fields

International Nuclear Information System (INIS)

Gorban', I.S.; Kozeeva, L.P.; Slobodyanyuk, A.V.; Shevchenko, V.A.

1987-01-01

The comparison of the electronic structure of Nd 3+ in CsNd(MoO 4 ) 2 and CsGd(MoO 4 ) 2 - Nd 3+ crystals is made. It is established that in these crystals the activator centers, mainly, of the certain type with the symmetry of the local environment C 2 are formed. The absorption spectra of self-activated CsNd(MoO 4 ) 2 crystal differ from spectra of CsGd(MoO 4 ) 2 - Nd 3+ by the presence of the vibrating structure. The Stark splittings of energy levels of Nd 3+ in the investigated crystalline matrices are more sensitive to the environment effect than the Zeeman ones. The ground state of Nd 3+ ion in CsNd(MoO 4 ) 2 and CsGd(MoO 4 ) 2 molybdates is characterized by the similar values of g-factors

The spectroscopy investigation of ZnWO{sub 4}:Tm{sup 3+} single crystal

Energy Technology Data Exchange (ETDEWEB)

Yang Fugui, E-mail: ruopiao@fjirsm.ac.cn [Department of Electronic Information Science, Fujian Jiangxia University, Fuzhou, Fujian 350108 (China); Tu Chaoyang [Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China)

2012-09-15

Highlights: Black-Right-Pointing-Pointer The spectroscopy and refractive index of single crystal ZnWO{sub 4}:Tm{sup 3+} are investigated systematically. Black-Right-Pointing-Pointer The Judd-Ofelt parameters are obtained. Black-Right-Pointing-Pointer The gain cross sections at {approx}2 {mu}m are estimated by reciprocity method (RM). Black-Right-Pointing-Pointer The laser operation at {approx}2 {mu}m is discussed. - Abstract: The single crystal ZnWO{sub 4}:Tm{sup 3+} has been grown by Czochralski method. The XRD, refractive index, absorption and fluorescence spectra are measured. The Judd-Ofelt parameters{Omega}{sub 2}, {Omega}{sub 4}, {Omega}{sub 6} are obtained to be 6.3 Multiplication-Sign 10{sup -20}, 1.3 Multiplication-Sign 10{sup -20}, 1.4 Multiplication-Sign 10{sup -20} cm{sup 2}, respectively. The fluorescence decay time of the {sup 3}H{sub 4} level is measured to be 0.113 ms and the quantum efficiency is 57%. The gain cross sections corresponding to {sup 3}F{sub 4}{yields}{sup 3}H{sub 6} transition at {approx}2 {mu}m are estimated by the reciprocity method (RM). The strong gain at {approx}2 {mu}m indicates that the ZnWO{sub 4}:Tm{sup 3+} crystal is a promising laser host for {approx}2 {mu}m laser.

Radiopurity of CaWO{sub 4} crystals for direct dark matter search with CRESST and EURECA

Energy Technology Data Exchange (ETDEWEB)

Muenster, Andrea [Physik Department E15, Technische Universitaet Muenchen, 85748 Garching (Germany); Collaboration: CRESST-Collaboration

2015-07-01

The direct dark matter search experiment CRESST uses scintillating CaWO{sub 4} single crystals as targets for possible WIMP recoils. A particle interaction in the crystal produces phonons as well as scintillation light. As the light signal is dependent on the kind of interacting particle, e{sup -}-recoils and α-decays mainly originating from intrinsic impurities of the crystal can be discriminated from nuclear recoils (e.g. due to possible WIMP scatterings). To achieve the best possible discrimination a high light output and a high radiopurity of the crystals are crucial. Since 2011 CaWO{sub 4} crystals are grown in the crystal lab of TU Munich. In this way we can directly influence the growth parameters and find a method to improve light output and radiopurity which is required by CRESST and the future tonne-scale multi-material experiment EURECA. In this talk we will discuss the investigated radiopurity of the raw materials WO{sub 3} and CaCO{sub 3} as well as of TUM-grown crystals which are currently taking data in CRESST II Phase 2.

Crystal structure of 1-ethylpyrazolo[3,4-d]pyrimidine-4(5H-thione

Directory of Open Access Journals (Sweden)

Mohammed El Fal

2014-09-01

Full Text Available In the title compound, C7H8N4S, the methyl C atom is displaced by 1.232 (7 Å from the mean plane of the pyrazolo[3,4-d]pyrimidine ring system (r.m.s. deviation = 0.007 Å. The N—N—C—Cm (m = methyl torsion angle is −60.3 (6°. In the crystal, molecules are linked by N—H...S hydrogen bonds, generating [010] chains, which are reinforced by C—H...N interactions. The chains are cross-linked by weak C—H...S hydrogen bonds, generating (001 sheets.

Crystallization of hepatocyte nuclear factor 4α (HNF4α) in complex with the HNF1α promoter element

Energy Technology Data Exchange (ETDEWEB)

Lu, Peng; Liu, Jianguo; Melikishvili, Manana; Fried, Michael G.; Chi, Young-In, E-mail: ychi@uky.edu [Department of Molecular and Cellular Biochemistry and Center for Structural Biology, University of Kentucky, Lexington, KY 40536 (United States)

2008-04-01

Sample preparation, characterization, crystallization and preliminary X-ray analysis are reported for the HNF4α–DNA binary complex. Hepatocyte nuclear factor 4α (HNF4α) is a member of the nuclear receptor superfamily that plays a central role in organ development and metabolic functions. Mutations on HNF4α cause maturity-onset diabetes of the young (MODY), a dominant monogenic cause of diabetes. In order to understand the molecular mechanism of promoter recognition and the molecular basis of disease-causing mutations, the recombinant HNF4α DNA-binding domain was prepared and used in a study of its binding properties and in crystallization with a 21-mer DNA fragment that contains the promoter element of another MODY gene, HNF1α. The HNF4α protein displays a cooperative and specific DNA-binding activity towards its target gene-recognition elements. Crystals of the complex diffract to 2.0 Å using a synchrotron-radiation source under cryogenic (100 K) conditions and belong to space group C2, with unit-cell parameters a = 121.63, b = 35.43, c = 70.99 Å, β = 119.36°. A molecular-replacement solution has been obtained and structure refinement is in progress. This structure and the binding studies will provide the groundwork for detailed functional and biochemical studies of the MODY mutants.

Crystallization of hepatocyte nuclear factor 4α (HNF4α) in complex with the HNF1α promoter element

International Nuclear Information System (INIS)

Lu, Peng; Liu, Jianguo; Melikishvili, Manana; Fried, Michael G.; Chi, Young-In

2008-01-01

Sample preparation, characterization, crystallization and preliminary X-ray analysis are reported for the HNF4α–DNA binary complex. Hepatocyte nuclear factor 4α (HNF4α) is a member of the nuclear receptor superfamily that plays a central role in organ development and metabolic functions. Mutations on HNF4α cause maturity-onset diabetes of the young (MODY), a dominant monogenic cause of diabetes. In order to understand the molecular mechanism of promoter recognition and the molecular basis of disease-causing mutations, the recombinant HNF4α DNA-binding domain was prepared and used in a study of its binding properties and in crystallization with a 21-mer DNA fragment that contains the promoter element of another MODY gene, HNF1α. The HNF4α protein displays a cooperative and specific DNA-binding activity towards its target gene-recognition elements. Crystals of the complex diffract to 2.0 Å using a synchrotron-radiation source under cryogenic (100 K) conditions and belong to space group C2, with unit-cell parameters a = 121.63, b = 35.43, c = 70.99 Å, β = 119.36°. A molecular-replacement solution has been obtained and structure refinement is in progress. This structure and the binding studies will provide the groundwork for detailed functional and biochemical studies of the MODY mutants

Electric conductivity and lattice disorder of PbMoO4 crystals

International Nuclear Information System (INIS)

Bollmann, W.

1980-01-01

From differential thermal analysis (DTA), thermal etching, perfectly reversable redox treatments and electric conductivity it is concluded that the Pb/Mo ratio of the PbMoO 4 crystals is always 1 and that phase transitions do not occur. Pb 3+ ions detectable by an absorption band at 435 nm cause a p-conductivity due to the reaction Pb 3+ reversible Pb ++ + e + . At elevated temperatures the p-conductivity increases with increasing oxygen partial pressure of the surrouding atmosphere. The influence of foreign ions on the concentration of ionic and electronic defects in PbMoO 4 , CaMoO 4 , PbO, and PbTiO 3 can be explained by an anti-Frenkel disorder of the oxygen ion sublattice. For PbMoO 4 crystals the mobility O -- ion vacancies and the free formation enthalpy of anti-Frenkel defects are found to be vsub(v) = 9160/T exp (-1.15 eV/kT) cm 2 K/Vs and gsub(AF) = 3.6 kT - 2.2 eV, respectively. (author)

Synthesis, crystal structure and DFT studies of N-(4-acetyl-5,5-dimethyl-4,5-dihydro-1,3,4-thiadiazol-2-yl)acetamide

Energy Technology Data Exchange (ETDEWEB)

Gautam, P.; Gautam, D.; Chaudhary, R. P., E-mail: rpchaudhary65@gmail.com [Sant Longowal Institute of Engineering and Technology, Department of Chemistry (India)

2013-12-15

The title compound N-(4-acetyl-5,5-dimethyl-4,5-dihydro-1,3,4-thiadiazol-2-yl)acetamide (III) was obtained from the reaction of 2-(propan-2-ylidene)hydrazinecarbothioamide (II) with acetic anhydride instead of formation of the desired thiosemcarbazide derivative of Meldrum acid. The structures of II and III were established by elemental analysis, IR, NMR, Mass and X-ray crystallographic studies. II crystallizes in triclinic system, sp. gr. P-bar1 Z = 2; III crystallizes in the monoclinic system, sp. gr. P2{sub 1}/c, Z = 8. Density functional theory (DFT) calculations have been carried out for III. {sup 1}H and {sup 13}C NMR of III has been calculated and correlated with experimental results.

Overexpression, crystallization and preliminary X-ray crystallographic analysis of erythronate-4-phosphate dehydrogenase from Pseudomonas aeruginosa.

Science.gov (United States)

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%.

Crystallization and preliminary crystallographic studies of the metalloglycoprotein esterase A4 using a baculovirus expression system

Energy Technology Data Exchange (ETDEWEB)

Hiraki, Toshiki [Protein Design Laboratory, Yokohama City University, 1-7-29 Suehiro, Tsurumi, Yokohama 230-0045 (Japan); Shibayama, Naoya [Department of Physiology, Division of Biophysics, Jichi Medical University, 3311-1 Yakushiji, Shimotsuke, Tochigi 329-0498 (Japan); Yoon, Young-Ho [Protein Design Laboratory, Yokohama City University, 1-7-29 Suehiro, Tsurumi, Yokohama 230-0045 (Japan); Yun, Kyung-Mook [Department of Physiology, Division of Biophysics, Jichi Medical University, 3311-1 Yakushiji, Shimotsuke, Tochigi 329-0498 (Japan); Hamamoto, Toshiro [Department of Biochemistry, Jichi Medical University, 3311-1 Yakushiji, Shimotsuke, Tochigi 329-0498 (Japan); Tame, Jeremy R. H.; Park, Sam-Yong, E-mail: park@tsurumi.yokohama-cu.ac.jp [Protein Design Laboratory, Yokohama City University, 1-7-29 Suehiro, Tsurumi, Yokohama 230-0045 (Japan)

2007-09-01

Esterase A4 (EA4) is a timer protein found in diapause eggs of the silkworm Bombyx mori. The gene for this metalloglycoprotein was cloned from B. mori eggs and expressed using a baculovirus expression system in silkworm pupae. Crystals of the purified protein have been grown that diffract to beyond 2.1 Å resolution at 100 K using synchrotron radiation. Esterase A4 (EA4) is a timer protein found in diapause eggs of the silkworm Bombyx mori. The gene for this metalloglycoprotein was cloned from B. mori eggs and expressed using a baculovirus expression system in silkworm pupae. Crystals of the purified protein have been grown that diffract to beyond 2.1 Å resolution at 100 K using synchrotron radiation. The protein crystals belong to space group P2{sub 1}, with unit-cell parameters a = 47.1, b = 73.9, c = 47.4 Å, β = 104.1°. With one dimer per asymmetric unit, the crystal volume per unit protein weight (V{sub M}) is 2.3 Å{sup 3} Da{sup −1} and the solvent content is 47%.

Crystal structure and spin state of mixed-crystals of iron with zinc and cobalt for the assembled complexes bridged by 1,3-bis(4-pyridyl)propanes

Energy Technology Data Exchange (ETDEWEB)

Dote, Haruka [Hiroshima University, Graduate School of Science (Japan); Nakashima, Satoru, E-mail: snaka@hiroshima-u.ac.jp [Hiroshima University, Natural Science Center for Basic Research and Development (Japan)

2012-03-15

Mixed crystals of cobalt and zinc were synthesized using 1,3-bis(4-pyridyl)propane (bpp) as bridging ligand and NCS{sup - } as anion. Red crystals and blue crystals were obtained. Powder X-ray diffraction patterns showed that the former is in 2D interpenetrated structure, while the latter has the same structure with Zn(NCS){sub 2}(bpp). Iron ion was introduced both into the red crystals and blue crystals of the mixed crystals of cobalt with zinc. {sup 57}Fe Moessbauer spectrum of the red crystals showed a main doublet of Fe{sup II} high-spin state at 78 K, while the spectrum of blue crystals did not show Fe{sup II} high-spin state at 78 K.

Crystal structure and spin state of mixed-crystals of iron with zinc and cobalt for the assembled complexes bridged by 1,3-bis(4-pyridyl)propanes

International Nuclear Information System (INIS)

Dote, Haruka; Nakashima, Satoru

2012-01-01

Mixed crystals of cobalt and zinc were synthesized using 1,3–bis(4–pyridyl)propane (bpp) as bridging ligand and NCS  −  as anion. Red crystals and blue crystals were obtained. Powder X-ray diffraction patterns showed that the former is in 2D interpenetrated structure, while the latter has the same structure with Zn(NCS) 2 (bpp). Iron ion was introduced both into the red crystals and blue crystals of the mixed crystals of cobalt with zinc. 57 Fe Mössbauer spectrum of the red crystals showed a main doublet of Fe II high-spin state at 78 K, while the spectrum of blue crystals did not show Fe II high-spin state at 78 K.

Lanthanide-doped NaScF4 nanoprobes: crystal structure, optical spectroscopy and biodetection.

Science.gov (United States)

Ai, Yu; Tu, Datao; Zheng, Wei; Liu, Yongsheng; Kong, Jintao; Hu, Ping; Chen, Zhuo; Huang, Mingdong; Chen, Xueyuan

2013-07-21

Trivalent lanthanide ions (Ln(3+))-doped inorganic nanoparticles (NPs) as potential luminescent bioprobes have been attracting tremendous interest because of their unique upconversion (UC) and downconversion (DC) luminescence properties. NaScF4, as an important host material, has been rarely reported and its crystal structure remains unclear. Herein, based on the single crystal X-ray diffraction, the space group of NaScF4 crystals was determined to be P31 containing multiple sites of Sc(3+) with crystallographic site symmetry of C1, which was verified by high-resolution photoluminescence spectroscopy of Eu(3+) at low temperature (10 K). Furthermore, monodisperse and size-controllable NaScF4:Ln(3+) NPs were synthesized via a facile thermal decomposition method. The biotinylated NaScF4:Er(3+)/Yb(3+) NPs were demonstrated for their applications as a heterogeneous UC luminescence bioprobe to detect avidin with a detection limit of 180 pM. After bioconjugation with amino-terminal fragment (ATF) of urokinase plasminogen activator (uPA), NaScF4:Ln(3+) NPs also exhibited specific recognition of cancer cells overexpressed with uPA receptor (uPAR, an important marker of tumor biology and metastasis), showing great potentials in tumor-targeted bioimaging.

Single crystal growth, electronic structure and optical properties of Cs2HgBr4

Science.gov (United States)

Lavrentyev, A. A.; Gabrelian, B. V.; Vu, V. T.; Shkumat, P. N.; Parasyuk, O. V.; Fedorchuk, A. O.; Khyzhun, O. Y.

2015-10-01

We report on successful synthesis of high-quality single crystal of cesium mercury tetrabromide, Cs2HgBr4, by using the vertical Bridgman-Stockbarger method as well as on studies of its electronic structure. For the Cs2HgBr4 crystal, we have recorded X-ray photoelectron spectra for both pristine and Ar+ ion-bombarded surfaces. Our data indicate that the Cs2HgBr4 single crystal surface is rather sensitive with respect to Ar+ ion-bombardment. In particular, such a treatment of the Cs2HgBr4 single crystal surface alters its elemental stoichiometry. To explore peculiarities of the energy distribution of total and partial densities of states within the valence band and the conduction band of Cs2HgBr4, we have made band-structure calculations based on density functional theory (DFT) employing the augmented plane wave+local orbitals (APW+lo) method as incorporated in the WIEN2k package. The APW+lo calculations allow for concluding that the Br 4p states make the major contributions in the upper portion of the valence band, while its lower portion is dominated by contributors of the Hg 5d and Cs 5p states. Further, the main contributors to the bottom of the conduction band of Cs2HgBr4 are the unoccupied Br p and Hg s states. In addition, main optical characteristics of Cs2HgBr4 such as dispersion of the absorption coefficient, real and imaginary parts of dielectric function, electron energy-loss spectrum, refractive index, extinction coefficient and optical reflectivity have been explored from the first-principles band-structure calculations.

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

Science.gov (United States)

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.

Synthesis, crystal growth and structure of Mg containing β-rhombohedral boron: MgB17.4

International Nuclear Information System (INIS)

Adasch, Volker; Hess, Kai-Uwe; Ludwig, Thilo; Vojteer, Natascha; Hillebrecht, Harald

2006-01-01

For the first time, single crystals of Mg containing β-rhombohedral boron MgB 17.4 were synthesised from the elements in a Mg/Cu melt at 1600deg. C. The crystal structure determined by the refinement of single crystal data (space group R-3m, a=10.991(2)A, c=24.161(4)A, 890 reflections, 123 variables, R 1 (F)=0.049, wR 2 (I)=0.122) improves and modifies the former structure model derived from earlier investigations on powder samples. Mg is located on four different positions with partial occupation. While the occupation of the sites D (53.3%), E (91%) and F (7.2%) is already known from other boron-rich borides related to β-rhombohedral boron, the occupation of the fourth position (18h, 6.7%) is observed for the first time. Two boron positions show partial occupation. The summation reveals the composition MgB 17.4 and Mg 5.85 B 101.9 , respectively, confirmed by WDX measurements. The single crystals of MgB 17.4 show the highest Mg content ever found. Preliminary measurements indicate no superconductivity

Growth Aspects, Structural and Optical Properties of 2-aminopyridinium 2,4 Dinitrophenolate Single Crystal

Directory of Open Access Journals (Sweden)

S. Reena Devi

2017-06-01

Full Text Available Organic single crystal of 2-aminopyridinium 2,4-dinitrophenolate single crystal was grown by slow evaporation technique. The cell parameters and space group (P were determined from single X-ray diffraction analysis. HRXRD studies ascertained the crystalline quality. UV-Visible and PL spectral studies revealed the emission in red region, transparency (75% cutoff wavelength around 440 nm respectively. The laser damage threshold of grown crystal was estimated by using Nd:YAG laser beam and these results were mutually related with specific heat capacity of the grown crystal. The third-order nonlinear optical parameters were estimated by Z-scan technique which is useful for optical applications.

Crystal structure of 3-{1′-[3,5-bis(trifluoromethylphenyl]ferrocenyl}-4-bromothiophene

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Elisabeth A. Poppitz

2014-10-01

Full Text Available The molecular structure of the title compound, [Fe(C9H6BrS(C13H7F6], consists of a ferrocene backbone with a bis(trifluoromethylphenyl group at one cyclopentadienyl ring and a thiophene heterocycle at the other cyclopentadienyl ring. The latter is disordered over two sets of sites in a 0.6:0.4 ratio. In the crystal structure, intramolecular π–π interactions between the thienyl and the phenyl substituent [centroid–centroid distance 3.695 (4 Å] and additional weak T-shaped π–π interactions between the thienyl and the phenyl-substituted cyclopentadienyl ring [4.688 (6 Å] consolidate the crystal packing.

Experimental investigation of 4-dimensional superspace crystals

International Nuclear Information System (INIS)

Rasing, T.; Janner, A.

1983-09-01

The symmetry of incommensurate crystals can be described by higher dimensional space groups in the so called superspace approach. The basic ideas are explained and used for showing that superspace groups provide an adequate frame for analyzing experimental results on incommensurate crystals

Crystal structure of human CRMP-4: correction of intensities for lattice-translocation disorder

Energy Technology Data Exchange (ETDEWEB)

Ponnusamy, Rajesh [Universidade Nova de Lisboa, Avenida da República, EAN, 2781-901 Oeiras (Portugal); Lebedev, Andrey A. [Research Complex at Harwell, STFC Rutherford Appleton Laboratory, Didcot OX11 0FA (United Kingdom); Pahlow, Steffen [University of Hamburg, Ohnhorststrasse 18, 22609 Hamburg (Germany); Lohkamp, Bernhard, E-mail: bernhard.lohkamp@ki.se [Karolinska Institutet, Tomtebodavägen 6, 4tr, 17177 Stockholm (Sweden); Universidade Nova de Lisboa, Avenida da República, EAN, 2781-901 Oeiras (Portugal)

2014-06-01

Crystals of human CRMP-4 showed severe lattice-translocation disorder. Intensities were demodulated using the so-called lattice-alignment method and a new more general method with simplified parameterization, and the structure is presented. Collapsin response mediator proteins (CRMPs) are cytosolic phosphoproteins that are mainly involved in neuronal cell development. In humans, the CRMP family comprises five members. Here, crystal structures of human CRMP-4 in a truncated and a full-length version are presented. The latter was determined from two types of crystals, which were either twinned or partially disordered. The crystal disorder was coupled with translational NCS in ordered domains and manifested itself with a rather sophisticated modulation of intensities. The data were demodulated using either the two-lattice treatment of lattice-translocation effects or a novel method in which demodulation was achieved by independent scaling of several groups of intensities. This iterative protocol does not rely on any particular parameterization of the modulation coefficients, but uses the current refined structure as a reference. The best results in terms of R factors and map correlation coefficients were obtained using this new method. The determined structures of CRMP-4 are similar to those of other CRMPs. Structural comparison allowed the confirmation of known residues, as well as the identification of new residues, that are important for the homo- and hetero-oligomerization of these proteins, which are critical to nerve-cell development. The structures provide further insight into the effects of medically relevant mutations of the DPYSL-3 gene encoding CRMP-4 and the putative enzymatic activities of CRMPs.

Crystal structure of human CRMP-4: correction of intensities for lattice-translocation disorder

International Nuclear Information System (INIS)

Ponnusamy, Rajesh; Lebedev, Andrey A.; Pahlow, Steffen; Lohkamp, Bernhard

2014-01-01

Crystals of human CRMP-4 showed severe lattice-translocation disorder. Intensities were demodulated using the so-called lattice-alignment method and a new more general method with simplified parameterization, and the structure is presented. Collapsin response mediator proteins (CRMPs) are cytosolic phosphoproteins that are mainly involved in neuronal cell development. In humans, the CRMP family comprises five members. Here, crystal structures of human CRMP-4 in a truncated and a full-length version are presented. The latter was determined from two types of crystals, which were either twinned or partially disordered. The crystal disorder was coupled with translational NCS in ordered domains and manifested itself with a rather sophisticated modulation of intensities. The data were demodulated using either the two-lattice treatment of lattice-translocation effects or a novel method in which demodulation was achieved by independent scaling of several groups of intensities. This iterative protocol does not rely on any particular parameterization of the modulation coefficients, but uses the current refined structure as a reference. The best results in terms of R factors and map correlation coefficients were obtained using this new method. The determined structures of CRMP-4 are similar to those of other CRMPs. Structural comparison allowed the confirmation of known residues, as well as the identification of new residues, that are important for the homo- and hetero-oligomerization of these proteins, which are critical to nerve-cell development. The structures provide further insight into the effects of medically relevant mutations of the DPYSL-3 gene encoding CRMP-4 and the putative enzymatic activities of CRMPs

Plasmonic enhancement in BiVO4 photonic crystals for efficient water splitting.

Science.gov (United States)

Zhang, Liwu; Lin, Chia-Yu; Valev, Ventsislav K; Reisner, Erwin; Steiner, Ullrich; Baumberg, Jeremy J

2014-10-15

Photo-electrochemical water splitting is a very promising and environmentally friendly route for the conversion of solar energy into hydrogen. However, the solar-to-H2 conversion efficiency is still very low due to rapid bulk recombination of charge carriers. Here, a photonic nano-architecture is developed to improve charge carrier generation and separation by manipulating and confining light absorption in a visible-light-active photoanode constructed from BiVO4 photonic crystal and plasmonic nanostructures. Synergistic effects of photonic crystal stop bands and plasmonic absorption are observed to operate in this photonic nanostructure. Within the scaffold of an inverse opal photonic crystal, the surface plasmon resonance is significantly enhanced by the photonic Bragg resonance. Nanophotonic photoanodes show AM 1.5 photocurrent densities of 3.1 ± 0.1 mA cm(-2) at 1.23 V versus RHE, which is among the highest for oxide-based photoanodes and over 4 times higher than the unstructured planar photoanode. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optical properties of Ni-doped MgGa2O4 single crystals grown by floating zone method

International Nuclear Information System (INIS)

Suzuki, Takenobu; Hughes, Mark; Ohishi, Yasutake

2010-01-01

The single crystal growth conditions and spectroscopic characterization of Ni-doped MgGa 2 O 4 with inverse-spinel structure crystal family are described. Single crystals of this material have been grown by floating zone method. Ni-doped MgGa 2 O 4 single crystals have broadband fluorescence in the 1100-1600 nm wavelength range, 1.6 ms room temperature lifetime, 56% quantum efficiency and 1.05x10 -21 cm 2 stimulated emission cross section at the emission peak. This new material is very promising for tunable laser applications covering the important optical communication and eye safe wavelength region.

Polarized spectral properties of Yb3+ : Li2Gd4(MoO4)7 crystal: a candidate for tunable and ultrashort pulse lasers

International Nuclear Information System (INIS)

Zhu Haomiao; Chen Yujin; Lin Yanfu; Gong Xinghong; Liao Jinsheng; Chen Xueyuan; Luo Zundu; Huang Yidong

2007-01-01

Detailed polarized spectral properties of a 3.2 at.% Yb 3+ : Li 2 Gd 4 (MoO 4 ) 7 crystal, including absorption cross-section, emission cross-section, up-conversion spectrum and intrinsic fluorescence lifetime, were investigated. The laser potentiality was also evaluated and the results show that this crystal is a good candidate for tunable and ultrashort pulse lasers

Growth and laser action of Yb: YVO4 crystals with low Yb doping concentration

Science.gov (United States)

Zhong, Degao; Teng, Bing; Li, Jianhong; Zhang, Shiming; Zhang, Bingtao; Wang, Chao; Tian, Xueping; Liu, Junhai

2012-11-01

Yb: YVO4 single crystals with low doping concentrations of Yb3+ less than 0.3 at% were grown using the Czochralski method. The polarized absorption spectra were measured at room temperature. Strong anisotropy exists in the absorption spectra, resulting in almost entirely different features for π-polarization and σ-polarization. The laser emission spectrum and relationship curve between the output power and absorbed pump power (Pabs) were measured. The continuous-wave laser action of Yb: YVO4 single crystal in a range of 1020.4-1026.3 nm was realized by using a high-power diode laser as the pump source.

Optical characteristics of BaGa{sub 2}S{sub 4}:Ho{sup 3+} and BaGa{sub 2}Se{sub 4}:Ho{sup 3+} single crystals

Energy Technology Data Exchange (ETDEWEB)

Choe, Sung-Hyu [Chosun University, Kwangju (Korea, Republic of); Jin, Moon-Seog [Dongshin University, Naju (Korea, Republic of); Kim, Wha-Tek [Chonnam National University, Kwangju (Korea, Republic of)

2005-11-15

BaGa{sub 2}S{sub 4}, BaGa{sub 2}S{sub 4}:Ho{sup 3+}, BaGa{sub 2}Se{sub 4}, and BaGa{sub 2}Se{sub 4}:Ho{sup 3+} single crystals were grown by using the chemical transport reaction method. The optical energy gaps of the single crystals were investigated in the temperature region from 11 K to 300 K. The temperature dependence of the optical energy gap was well fitted by the Varshni equation. Two broad emission bands were observed in the photoluminescence spectra of the single crystals. These bands were attributed to donor-acceptor pair recombinations. Sharp emission peaks were observed in the BaGa{sub 2}S{sub 4}:Ho{sup 3+} and the BaGa{sub 2}Se{sub 4}:Ho{sup 3+} single crystals and were assigned to radiation recombination between split Stark levels of Ho{sup 3+}.

Microwave-Assisted Synthesis and Crystal Structure of Oxo(diperoxo(4,4'-di-tert-butyl-2,2'-bipyridine-molybdenum(VI

Directory of Open Access Journals (Sweden)

Alírio E. Rodrigues

2009-09-01

Full Text Available The oxodiperoxo complex MoO(O22(tbbpy (tbbpy = 4,4'-di-tert-butyl-2,2'- bipyridine was isolated from the reaction of MoO2Cl2(tbbpy in water under microwaveassisted heating at 120 ºC for 4 h. The structure of the oxodiperoxo complex was determined by single crystal X-ray diffraction. The MoVI centre is seven-coordinated with a geometry which strongly resembles a highly distorted bipyramid. Individual MoO(O22(tbbpy complexes are interdigitated along the [010] direction to form a column. The crystal structure is formed by the close packing of the columnar-stacked complexes. Interactions between neighbouring columns are essentially of van der Waals type mediated by the need to effectively fill the available space.

Spin dynamics, electronic, and thermal transport properties of two-dimensional CrPS4 single crystal

Science.gov (United States)

Pei, Q. L.; Luo, X.; Lin, G. T.; Song, J. Y.; Hu, L.; Zou, Y. M.; Yu, L.; Tong, W.; Song, W. H.; Lu, W. J.; Sun, Y. P.

2016-01-01

2-Dimensional (2D) CrPS4 single crystals have been grown by the chemical vapor transport method. The crystallographic, magnetic, electronic, and thermal transport properties of the single crystals were investigated by the room-temperature X-ray diffraction, electrical resistivity ρ(T), specific heat CP(T), and the electronic spin response (ESR) measurements. CrPS4 crystals crystallize into a monoclinic structure. The electrical resistivity ρ(T) shows a semiconducting behavior with an energy gap Ea = 0.166 eV. The antiferromagnetic transition temperature is about TN = 36 K. The spin flipping induced by the applied magnetic field is observed along the c axis. The magnetic phase diagram of CrPS4 single crystal has been discussed. The extracted magnetic entropy at TN is about 10.8 J/mol K, which is consistent with the theoretical value R ln(2S + 1) for S = 3/2 of the Cr3+ ion. Based on the mean-field theory, the magnetic exchange constants J1 and Jc corresponding to the interactions of the intralayer and between layers are about 0.143 meV and -0.955 meV are obtained based on the fitting of the susceptibility above TN, which agree with the results obtained from the ESR measurements. With the help of the strain for tuning the magnetic properties, monolayer CrPS4 may be a promising candidate to explore 2D magnetic semiconductors.

Comparative study of optical and scintillation properties of YVO{sub 4}, (Lu{sub 0.5}Y{sub 0.5})VO{sub 4}, and LuVO{sub 4} single crystals

Energy Technology Data Exchange (ETDEWEB)

Fujimoto, Yutaka, E-mail: fuji-you@tagen.tohoku.ac.j [IMRAM, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan); Yanagida, Takayuki; Yokota, Yuui; Chani, Valery [IMRAM, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan); Kochurikhin, Vladimir V. [General Physics Institute, 38 Vavilov Street, 119991, Federation, Moscow (Russian Federation); Yoshikawa, Akira [IMRAM, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan); NICHe, Tohoku University, 6-6-10 Aoba, Aramaki, Aoba-ku, Sendai 980-8579 (Japan)

2011-04-11

Optical and scintillation properties of YVO{sub 4}, (Lu{sub 0.5}Y{sub 0.5})VO{sub 4}, and LuVO{sub 4} single crystals grown by the Czochralski (CZ) method with RF heating system are compared. All vanadate crystals show high transmittance ({approx}80%) in the 400-900 nm wavelength range. In both photo- and radio-luminescence spectra, intense peak around 400-500 nm, which was ascribed to the transition from triplet state of VO{sub 4}{sup 3-}, was clearly observed. The main decay time component was about 38 {mu}s (YVO{sub 4}), 18 {mu}s ((Lu{sub 0.5}Y{sub 0.5})VO{sub 4}), and 17 {mu}s (LuVO{sub 4}) under 340 nm excitation. The scintillation light yields of YVO{sub 4}, (Lu{sub 0.5}Y{sub 0.5})VO{sub 4}, and LuVO{sub 4} crystals (obtained from the {sup 137}Cs excited pulse height spectra) were evaluated to be about 11,200, 10,700, and 10,300 ph/MeV, respectively.

Synthesis, Crystal Structure and Anti-ischaemic Activity of (E)-1-{4 ...

African Journals Online (AJOL)

NICO

Mr = 476.98) (5) was synthesized and studied by the single crystal X-ray diffraction method. Its structure was ... The reaction of cinnamic acid chloride with 1-[bis(4-methoxy- .... Displacement ellipsoids are drawn at the 70 % probability level.

The effect of pressure on the conductivity behavior of the (NH4)3H(SeO4)2 superprotonic crystal

Science.gov (United States)

Lindner, Ł.; Zdanowska-Frączek, M.; Pawłowski, A.; Frączek, Z. J.; Masłowski, T.

2017-07-01

The impedance spectra of (NH4)3 H(SeO4)2 in low and high-conductive phases under various thermodynamic conditions were analyzed. The measurements were performed by the ac admittance technique along the trigonal c axis of the crystal, i.e., along the direction perpendicular to the plane in which, in the superionic phases, a dynamically disordered H-bond network was formed. Activation energies and activation volumes were calculated for different phases of the (NH4)3 H(SeO4)2 crystal from the baric dependencies of dc conductivity and they were correlated with pressure coefficients of the phase transitions. The experimental results were analyzed within the classical hopping model, in terms of the strong proton-phonon coupling and polaronic effect.

Synthesis and crystal structure of the quaternary compound AgFe{sub 2}GaTe{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Delgado, Gerzon E., E-mail: gerzon@ula.ve [Laboratorio de Cristalografía, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101 (Venezuela, Bolivarian Republic of); Quintero, Eugenio; Tovar, Rafael; Grima-Gallardo, Pedro; Quintero, Miguel [Centro de Estudio de Semiconductores, Departamento de Física, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101 (Venezuela, Bolivarian Republic of)

2014-11-15

Highlights: • New quaternary compound. • Synthesis from solid state reaction. • Crystal structure. • Rietveld refinement. - Abstract: The crystal structure of the quaternary compound AgFe{sub 2}GaTe{sub 4}, belonging to the system I–II{sub 2}–III–VI{sub 4}, was characterized by Rietveld refinement using X-ray powder diffraction data. The powder pattern was composed by 84.5% of the principal phase AgFe{sub 2}GaTe{sub 4} and 15.5% of the secondary phase FeTe. This material crystallizes with stannite structure in the tetragonal space group I-42m (N° 121), Z = 2, unit cell parameters a = 6.3409(2) Å, c = 12.0233(4) Å, V = 483.42(3) Å{sup 3}, and is isostructural with CuFe{sub 2}InSe{sub 4}.

Ferromagnetism in proton irradiated 4H-SiC single crystal

Directory of Open Access Journals (Sweden)

Ren-Wei Zhou

2015-04-01

Full Text Available Room-temperature ferromagnetism is observed in proton irradiated 4H-SiC single crystal. An initial increase in proton dose leads to pronounced ferromagnetism, accompanying with obvious increase in vacancy concentration. Further increase in irradiation dose lowers the saturation magnetization with the decrease in total vacancy defects due to the defects recombination. It is found that divacancies are the mainly defects in proton irradiated 4H-SiC and responsible for the observed ferromagnetism.

Crystal structure of RbCe(SeO4)2 · 5H2O

International Nuclear Information System (INIS)

Ovanesyan, S.M.; Iskhakova, L.D.; Trunov, V.K.

1987-01-01

RbTR(SeO 4 ) 2 x5H 2 O TR=La-Pr are synthesized. Crystal structure of RbCe(SeO 4 ) 2 x5H 2 O is studied. Monoclinic unit parameters are: a=7,200(2), b=8,723(1), c=19,258(6) A, Β=90,88(2), ρ (calc) =3,304 sp.gr. P2 1 /c. Within the structure the Ce nine vertex cages are united by Se(1)- and Se(2)-tetrahedrons in (Ce(SeO 4 ) 2 (H 2 O) 5 ) 2 ∞ n- layers. Some crystal structure regularities of the laminated MTR(EO 4 ) 2 xnH 2 O (M=NH 4 ,K,Rb,Cs; TR=La-Ln, E=S,Se) are considered

A Dual-Crystal Cavity Ho,Tm:GdVO4 Laser

International Nuclear Information System (INIS)

Zhu Guo-Li; Ju You-Lun; Yao Bao-Quan; Wang Yue-Zhu

2012-01-01

We report a 31.2 W cw diode-pumped cryogenic Ho(0.4at.%),Tm(4at.%):GdVO 4 laser in a dual-crystal cavity. The pumping sources are two fiber-coupled laser diodes with a fiber core diameter of 0.4 mm, both of which can supply 42 W near 802 nm. With an incident pump power of 70.3 W at 802.4 nm, a cw output power of 31.2 W at 2.05 μm is attained, corresponding to an optical-to-optical conversion efficiency of 44.4%. The M 2 factor is measured as ∼1.3 under an output power of 20 W. (fundamental areas of phenomenology(including applications))

Synthesis, characterization, and crystal structure of 2-amino-7-methyl-5-oxo-4-phenyl-4,5-dihydropyrano[3,2-c] pyran-3-carbonitrile

Energy Technology Data Exchange (ETDEWEB)

Sharma, S. [University of Jammu, X-ray Crystallography Laboratory, Post-Graduate Department of Physics and Electronics (India); Banerjee, B.; Brahmachari, G. [Visva-Bharati (a Central University), Laboratory of Natural Products & Organic Synthesis, Department of Chemistry (India); Kant, Rajni; Gupta, V. K., E-mail: vivek-gupta2k2@hotmail.com [University of Jammu, X-ray Crystallography Laboratory, Post-Graduate Department of Physics and Electronics (India)

2015-12-15

2-Amino-7-methyl-5-oxo-4-phenyl-4,5-dihydropyrano[3,2-c] pyran-3-carbonitrile, C{sub 16}H{sub 12}N{sub 2}O{sub 3} is synthesized via one-pot multi-component reaction at room temperature using commercially available urea as inexpensive and environmentally benign organo-catalyst. Its structure is determined by single-crystal X-ray diffraction technique The crystals are monoclinic, a = 10.7357(12), b = 8.7774(8), c = 15.0759(16) Å, β = 103.575(11)°, Z = 4, sp. gr. P2{sub 1}/n, R = 0.0551 for 1696 observed reflections. The crystal structure is stabilized by N–H···N, C–H···O, and C–H···π interactions.

Crystal phase-based epitaxial growth of hybrid noble metal nanostructures on 4H/fcc Au nanowires

Science.gov (United States)

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.

Inhomogeneous strain induced by fast neutron irradiation in NaKSO4 crystals

International Nuclear Information System (INIS)

Kandil, S.H.; El Gamal, M.A.; El Khatib, A.; El Wahidy, E.F.

1987-06-01

The effect of fast neutron irradiation on the thermal properties of NaKSO 4 crystals was studied around the phase transition temperature T c =453 K. The thermal expansion coefficient as well as the phase transition temperature were found to be dependent upon the irradiation dose. The specific heat, C p , showed multiple peaks in the phase transition temperature region. An explanation of this behaviour was based on the induced inhomogeneous strain in the crystal casued by the neutron irradiation process. (author). 10 refs, 3 figs

Accurate X-ray diffraction studies of KTiOPO{sub 4} single crystals doped with niobium

Energy Technology Data Exchange (ETDEWEB)

Novikova, N. E., E-mail: natnov@ns.crys.ras.ru; Sorokina, N. I.; Alekseeva, O. A.; Verin, I. A. [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Crystallography and Photonics Federal Scientific Research Center (Russian Federation); Kharitonova, E. P.; Orlova, E. I.; Voronkova, V. I. [Moscow State University, Faculty of Physics (Russian Federation)

2017-01-15

Single crystals of potassium titanyl phosphate doped with 4% of niobium (КТР:4%Nb) and 6% of niobium (KTP:6%Nb) are studied by accurate X-ray diffraction at room temperature. The niobium atoms are localized near the Ti1 and Ti2 atomic positions, and their positions are for the first time refined independent of the titanium atomic positions. Maps of difference electron density in the vicinity of K1 and K2 atomic positions are analyzed. It is found that in the structure of crystal КТР:4%Nb, additional positions of K atoms are located farther from the main positions and from each other than in КТР and KTP:6%Nb crystals. The nonuniform distribution of electron density found in the channels of the КТР:4%Nb structure is responsible for ~20% increase in the signal of second harmonic generation.

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

Science.gov (United States)

Prabakaran, R.; Subramanian, P.

2018-04-01

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

Photoresponse of CsPbBr3 and Cs4PbBr6 Perovskite Single Crystals.

Science.gov (United States)

Cha, Ji-Hyun; Han, Jae Hoon; Yin, Wenping; Park, Cheolwoo; Park, Yongmin; Ahn, Tae Kyu; Cho, Jeong Ho; Jung, Duk-Young

2017-02-02

High-quality and millimeter-sized perovskite single crystals of CsPbBr 3 and Cs 4 PbBr 6 were prepared in organic solvents and studied for correlation between photocurrent generation and photoluminescence (PL) emission. The CsPbBr 3 crystals, which have a 3D perovskite structure, showed a highly sensitive photoresponse and poor PL signal. In contrast, Cs 4 PbBr 6 crystals, which have a 0D perovskite structure, exhibited more than 1 order of magnitude higher PL intensity than CsPbBr 3 , which generated an ultralow photoresponse under illumination. Their contrasting optoelectrical characteristics were attributed to different exciton binding energies, induced by coordination geometry of the [PbBr 6 ] 4- octahedron sublattices. This work correlated the local structures of lead in the primitive perovskite and its derivatives to PL spectra as well as photoconductivity.

Crystal structures of lazulite-type oxidephosphates TiIIITiIV3O3(PO4)3 and MIII4TiIV27O24(PO4)24 (MIII=Ti, Cr, Fe)

International Nuclear Information System (INIS)

Schoeneborn, M.; Glaum, R.; Reinauer, F.

2008-01-01

Single crystals of the oxidephosphates Ti III Ti IV 3 O 3 (PO 4 ) 3 (black), Cr III 4 Ti IV 27 O 24 (PO 4 ) 24 (red-brown, transparent), and Fe III 4 Ti IV 27 O 24 (PO 4 ) 24 (brown) with edge-lengths up to 0.3 mm were grown by chemical vapour transport. The crystal structures of these orthorhombic members (space group F2dd ) of the lazulite/lipscombite structure family were refined from single-crystal data [Ti III Ti IV 3 O 3 (PO 4 ) 3 : Z=24, a=7.3261(9) A, b=22.166(5) A, c=39.239(8) A, R 1 =0.029, wR 2 =0.084, 6055 independent reflections, 301 variables; Cr III 4 Ti IV 27 O 24 (PO 4 ) 24 : Z=1, a=7.419(3) A, b=21.640(5) A, c=13.057(4) A, R 1 =0.037, wR 2 =0.097, 1524 independent reflections, 111 variables; Fe III 4 Ti IV 27 O 24 (PO 4 ) 24 : Z=1, a=7.4001(9) A, b=21.7503(2) A, c=12.775(3) A, R 1 =0.049, wR 2 =0.140, 1240 independent reflections, 112 variables). For Ti III Ti IV O 3 (PO 4 ) 3 a well-ordered structure built from dimers [Ti III,IV 2 O 9 ] and [Ti IV,IV 2 O 9 ] and phosphate tetrahedra is found. The metal sites in the crystal structures of Cr 4 Ti 27 O 24 (PO 4 ) 24 and Fe 4 Ti 27 O 24 (PO 4 ) 24 , consisting of dimers [M III Ti IV O 9 ] and [Ti IV,IV 2 O 9 ], monomeric [Ti IV O 6 ] octahedra, and phosphate tetrahedra, are heavily disordered. Site disorder, leading to partial occupancy of all octahedral voids of the parent lipscombite/lazulite structure, as well as splitting of the metal positions is observed. According to Guinier photographs Ti III 4 Ti IV 27 O 24 (PO 4 ) 24 (a=7.418(2) A, b=21.933(6) A, c=12.948(7) A) is isotypic to the oxidephosphates M III 4 Ti IV 27 O 24 (PO 4 ) 24 (M III : Cr, Fe). The UV/vis spectrum of Cr 4 Ti 27 O 24 (PO 4 ) 24 reveals a rather small ligand-field splitting Δ o =14,370 cm -1 and a very low nephelauxetic ratio β=0.72 for the chromophores [Cr III O 6 ] within the dimers [Cr III Ti IV O 9 ]. - Graphical abstract: Single crystals of the oxidephosphates Ti III Ti IV 3 O 3 (PO 4 ) 3 (black), Cr III 4 Ti IV 27 O

High-pressure synthesis and crystal structure of α-Y{sub 2}B{sub 4}O{sub 9}

Energy Technology Data Exchange (ETDEWEB)

Schmitt, Martin K.; Huppertz, Hubert [Innsbruck Univ. (Austria). Inst. fuer Allgemeine, Anorganische und Theoretische Chemie

2017-07-01

α-Y{sub 2}B{sub 4}O{sub 9} was synthesized in a high-pressure/high-temperature experiment at 12.3 GPa/1020 C. The crystal structure has been determined via single-crystal X-ray diffraction. α-Y{sub 2}B{sub 4}O{sub 9} is isotypic to the lanthanide borates α-Ln{sub 2}B{sub 4}O{sub 9} (Ln = Sm-Ho) and crystallizes in the monoclinic space group C2/c (no. 15) with the following lattice parameters: a = 25.084(2), b = 4.3913(2), c = 24.726(2) Aa, and β = 99.97(1) . The compound was further characterized via X-ray powder diffraction as well as IR and Raman spectroscopy.

Molecular and crystal structure of 2-((E)-[(4-Methylphenyl)imino]methyl)-4-nitrophenol: A redetermination

International Nuclear Information System (INIS)

Kaynar, Nihal Kan; Tanak, Hasan; Şahin, Songul; Dege, Necmi; Ağar, Erbil; Yavuz, Metin

2016-01-01

The crystal structure of the title compound, C_1_4H_1_2N_2O_3, was recently determined as a mixture of its neutral (OH containing) and zwitterionic (NH containing) forms, in a 0.60 (4): 0.40 (4) ratio using the X-ray determination. In this study, the title compound has been characterized by FT-IR and X-ray diffraction. The redetermination showed that the title compound has only enol (OH) form because of lack of the NH stretching vibration in FT-IR spectrum. In addition, the molecular structure and tautomerism of the title compound have been discussed.

High-Pressure Phase Relations and Crystal Structures of Postspinel Phases in MgV2O4, FeV2O4, and MnCr2O4: Crystal Chemistry of AB2O4 Postspinel Compounds.

Science.gov (United States)

Ishii, Takayuki; Sakai, Tsubasa; Kojitani, Hiroshi; Mori, Daisuke; Inaguma, Yoshiyuki; Matsushita, Yoshitaka; Yamaura, Kazunari; Akaogi, Masaki

2018-06-04

We have investigated high-pressure, high-temperature phase transitions of spinel (Sp)-type MgV 2 O 4 , FeV 2 O 4 , and MnCr 2 O 4 . At 1200-1800 °C, MgV 2 O 4 Sp decomposes at 4-7 GPa into a phase assemblage of MgO periclase + corundum (Cor)-type V 2 O 3 , and they react at 10-15 GPa to form a phase with a calcium titanite (CT)-type structure. FeV 2 O 4 Sp transforms to CT-type FeV 2 O 4 at 12 GPa via decomposition phases of FeO wüstite + Cor-type V 2 O 3 . MnCr 2 O 4 Sp directly transforms to the calcium ferrite (CF)-structured phase at 10 GPa and 1000-1400 °C. Rietveld refinements of CT-type MgV 2 O 4 and FeV 2 O 4 and CF-type MnCr 2 O 4 confirm that both the CT- and CF-type structures have frameworks formed by double chains of edge-shared B 3+ O 6 octahedra (B 3+ = V 3+ and Cr 3+ ) running parallel to one of orthorhombic cell axes. A relatively large A 2+ cation (A 2+ = Mg 2+ , Fe 2+ , and Mn 2+ ) occupies a tunnel-shaped space formed by corner-sharing of four double chains. Effective coordination numbers calculated from eight neighboring oxygen-A 2+ cation distances of CT-type MgV 2 O 4 and FeV 2 O 4 and CF-type MnCr 2 O 4 are 5.50, 5.16, and 7.52, respectively. This implies that the CT- and CF-type structures practically have trigonal prism (six-coordinated) and bicapped trigonal prism (eight-coordinated) sites for the A 2+ cations, respectively. A relationship between cation sizes of VIII A 2+ and VI B 3+ and crystal structures (CF- and CT-types) of A 2+ B 2 3+ O 4 is discussed using the above new data and available previous data of the postspinel phases. We found that CF-type A 2+ B 2 3+ O 4 crystallize in wide ionic radius ranges of 0.9-1.4 Å for VIII A 2+ and 0.55-1.1 Å for VI B 3+ , whereas CT-type phases crystallize in very narrow ionic radius ranges of ∼0.9 Å for VIII A 2+ and 0.6-0.65 Å for VI B 3+ . This would be attributed to the fact that the tunnel space of CT-type structure is geometrically less flexible due to the smaller coordination

Fluid evolution and ore genesis of the Dalingshang deposit, Dahutang W-Cu ore field, northern Jiangxi Province, South China

Science.gov (United States)

Peng, Ning-Jun; Jiang, Shao-Yong; Xiong, Suo-Fei; Pi, Dao-Hui

2018-02-01

The Dalingshang W-Cu deposit is located in the North section of the Dahutang ore field, northern Jiangxi Province, South China. Vein- and breccia-style tungsten-copper mineralization is genetically associated with Mesozoic S-type granitic rocks. Infrared and conventional microthermometric studies of both gangue and ore minerals show that the homogenization temperatures for primary fluid inclusions in wolframite ( 340 °C) are similar to those in scheelite ( 330 °C), but about 40 °C higher than those of apatite ( 300 °C) and generally 70 °C higher than those in coexisting quartz ( 270 °C). Laser Raman analysis identifies CH4 and N2 without CO2 in fluid inclusions in scheelite and coexisting quartz, while fluid inclusions in quartz of the sulfide stage have variable CO2 content. The ore-forming fluids overall are characterized by high- to medium-temperature, low-salinity, CH4, N2, and/or CO2-bearing aqueous fluids. Chalcopyrite, muscovite, and sphalerite are the most abundant solids recognized in fluid inclusions from different ores. The H-O-S-Pb isotope compositions favor a dominantly magmatic origin for ores and fluids, while some depleted δ34S values (- 14.4 to - 0.9‰) of sulfides from the sulfide stage are most likely produced by an increase of oxygen fugacity, possibly caused by inflow of oxidized meteoric waters. The microthermometric data also indicate that a simple cooling process formed early scheelite and wolframite. However, increasing involvement of meteoric waters and fluid mixing may trigger a successive deposition of base metal sulfides. Fluid-rock interaction was critical for scheelite mineralization as indicated by in-situ LA-ICP-MS analysis of trace elements in scheelite.

Crystal structure of 1,4-bis(3-ammoniopropylpiperazine-1,4-diium bis[dichromate(VI

Directory of Open Access Journals (Sweden)

S. Vetrivel

2016-05-01

Full Text Available The asymmetric unit of the organic–inorganic title salt, (C10H28N4[Cr2O7]2, comprises one half of an 1,4-bis(3-ammoniopropylpiperazinediium cation (the other half being generated by the application of inversion symmetry and a dichromate anion. The piperazine ring of the cation adopts a chair conformation, and the two CrO4 tetrahedra of the anion are in an almost eclipsed conformation. In the crystal, the cations and anions form a layered arrangement parallel to (001. N—H...O hydrogen bonds between the cations and anions and additional C—H...O interactions lead to the formation of a three-dimensional network structure.

Electron excitations in BeAl2O4, Be2SiO4 and Be3Al2Si6O18 crystals

International Nuclear Information System (INIS)

Ivanov, V.Yu.; Pustovarov, V.A.; Shlygin, E.S.; Korotaev, A.V.; Kruzhalov, A.V.

2005-01-01

Low-temperature (T = 7 K) time-resolved selectively photoexcited luminescence spectra (2-6 eV) and luminescence excitation spectra (8-35 eV) of wide-bandgap chrysoberyl BeAl 2 O 4 , phenacite Be 2 SiO 4 , and beryl Be 3 Al 2 Si 6 O 18 crystals have been studied using time-resolved VUV spectroscopy. Both the intrinsic luminescence of the crystals and the luminescence associated with structural defects were assigned. Energy transfer to impurity luminescence centers in alexandrite and emerald was investigated. Luminescence characteristics of stable crystal lattice defects were probed by 3.6-MeV accelerated helium ion beams [ru

Improvement of optical properties and radiation hardness of NaBi(WO sub 4) sub 2 Cherenkov crystals

CERN Document Server

Zadneprovski, B I; Polyansky, E V; Devitsin, E G; Kozlov, V A; Potashov, S Yu; Terkulov, A R

2002-01-01

On the basis of the data on melt evaporation while growing NaBi(WO sub 4) sub 2 Cherenkov crystals, the formation of nonstoichiometry and most probable types of dot defects of the crystals have been considered. The influence of melt nonstoichiometry and doping with Sc on optical transmission and radiation hardness of the crystals has been experimentally investigated. The surplus of WO sub 3 has been established to increase optical transmission and radiation hardness and lack of Bi sub 2 O sub 3 in the melt to reduce radiation hardness. Sc doping is shifting the absorption edge to UV region by 30-35 nm and is increasing radiation hardness of the crystals about three-fold. Analytical estimations give the increase of the number of Cherenkov photons by a factor of 1.3, which leads to an improvement of the energy resolution of a calorimeter based on NaBi(WO sub 4) sub 2 :Sc crystals compared with undoped NaBi(WO sub 4) sub 2 of approximately 15%.

Growth and properties of M2-xCexCuO4+d single crystals

International Nuclear Information System (INIS)

Matacotta, F.C.; Morales de La Garza, L.; Nevriva, M.; Nardin, G.; Randaccio, L.; Zangrando, E.

1989-10-01

The M 2-x Ce x CuO 4+d crystals where M is a rare earth ion (like Nd, Pr etc.) were prepared by a modified flux method, their structure has been investigated by scanning electron microscopy and energy dispersive X-ray analysis and the electrical resistivity was measured on a number of crystals. 5 refs, 3 figs, 3 tabs

Synthesis, crystal structure and electrochemical properties of the manganese-doped LiNaFe[PO{sub 4}]F materials

Energy Technology Data Exchange (ETDEWEB)

Ben Yahia, Hamdi, E-mail: benyahia.hamdi@aist.go.jp; Shikano, Masahiro, E-mail: shikano.masahiro@aist.go.jp; Sakaebe, Hikari; Kobayashi, Hironori

2013-08-15

The new compounds LiNaFe{sub 1−x}Mn{sub x}[PO{sub 4}]F (x ≤ 1/4) were synthesized by a solid state reaction route. The crystal structure of LiNaFe{sub 3/4}Mn{sub 1/4}[PO{sub 4}]F was determined from single crystal X-ray diffraction data. LiNaFe{sub 3/4}Mn{sub 1/4}[PO{sub 4}]F crystallizes with the Li{sub 2}Ni[PO{sub 4}]F-type structure, space group Pnma, a = 10.9719(13), b = 6.3528(7), c = 11.4532(13) Å, V = 798.31(16) Å{sup 3}, and Z = 8. The structure consists of edge-sharing (Fe{sub 3/4}Mn{sub 1/4})O{sub 4}F{sub 2} octahedra forming (Fe{sub 3/4}Mn{sub 1/4})FO{sub 3} chains running along the b-axis. These chains are interlinked by PO{sub 4} tetrahedra forming a three-dimensional framework with the tunnels and the cavities filled by the well-ordered sodium and lithium atoms, respectively. The manganese-doped phases show poor electrochemical behavior comparing to the iron pure phase LiNaFe[PO{sub 4}]F. - Highlights: • We investigated the synthesis of LiNaFe{sub 1−x}Mn{sub x}[PO{sub 4}]F by solid state reaction. • We demonstrated that a solid solution exist only for x ≤ 1/4. • We solved the crystal structure of LiNaFe{sub 3/4}Mn{sub 1/4}[PO{sub 4}]F using single crystal data. • We studied the electrochemical performances of LiNaFe{sub 1−x}Mn{sub x}[PO{sub 4}]F. • The Mn-doped phases have poor electrochemical performances comparing to LiNaFe[PO{sub 4}]F.

Structural, vibrational and luminescence properties of the (1−x)CaWO{sub 4}−xCdWO{sub 4} system

Energy Technology Data Exchange (ETDEWEB)

Taoufyq, A. [Institut Matériaux Microélectronique et Nanosciences de Provence, Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 83957, La Garde (France); Laboratoire Matériaux et Environnement LME, Faculté des Sciences, Université Ibn Zohr, BP 8106, Cité Dakhla, Agadir, Maroc (Morocco); CEA/DEN, Département d’Études des Réacteurs, Laboratoire Dosimétrie Capteurs Instrumentation, CEA Cadarache, 13108, Saint-Paul-lez-Durance (France); Société CESIGMA, Signals and Systems, 1576 Chemin de La Planquette, 83130 La Garde (France); Guinneton, F.; Valmalette, J-C.; Arab, M. [Institut Matériaux Microélectronique et Nanosciences de Provence, Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 83957, La Garde (France); Benlhachemi, A.; Bakiz, B. [Laboratoire Matériaux et Environnement LME, Faculté des Sciences, Université Ibn Zohr, BP 8106, Cité Dakhla, Agadir, Maroc (Morocco); Villain, S. [Institut Matériaux Microélectronique et Nanosciences de Provence, Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 83957, La Garde (France); and others

2014-11-15

In the present work, we investigate the structural, microstructural, vibrational and luminescence properties of the system (1−x)CaWO{sub 4}−xCdWO{sub 4} with x ranging between 0 and 1. Polycrystalline samples were elaborated using a coprecipitation technique followed by thermal treatment at 1000 °C. The samples were then characterized using X-ray diffraction, scanning electron microscopy, Raman spectroscopy and luminescence analyses. X-ray diffraction profile analyses using Rietveld method showed that two kinds of solid solutions Ca{sub 1−x}Cd{sub x}WO{sub 4} having scheelite and wolframite structures, with respectively tetragonal and monoclinic crystal cells, were observed, with a biphasic system for compositions x=0.6 and 0.7. The scanning electron microscopy experiments showed a complex evolution of morphologies and crystallite sizes as x increased. The vibration modes of Raman spectra were characteristic of composition-dependent disordered solid solutions with decreasing wavenumbers as x increased. Luminescence experiments were performed under UV-laser light irradiation. The energies of emission bands increased linearly with cadmium composition x. The integrated intensity of luminescence reached a maximum value for the substituted wolframite phase with composition x=0.8. - Graphical abstract: Luminescence on UV excitation (364.5 nm) of (1−x)CaWO{sub 4−x}CdWO{sub 4} system, elaborated from coprecipitation technique at 1000 °C, with 04} polycrystalline phases with 0≤x≤0.5. (b) Maximum of luminescence intensity for the composition x=0.8. - Highlights: • Solid solutions Ca{sub 1−x}Cd{sub x}WO{sub 4} are elaborated from coprecipitation technique. • The structures of two types of solid solutions are refined using Rietveld method. • A maximum of luminescence is obtained for an intermediate composition x=0.8.

Tuning crystal field symmetry of hexagonal NaY0.92Yb0.05Er0.03F4 by Ti4+ codoping for high-performance upconversion

International Nuclear Information System (INIS)

Yu, Han; Huang, Qingming; Ma, En; Zhang, Xinqi; Yu, Jianchang

2014-01-01

Highlights: • Upconversion emission of Er 3+ was obviously enhanced by Ti 4+ codoped in NaYF 4 . • The upconversion luminescence lifetime was also obviously prolonged. • Na + could be induced to occupy Y 3+ sites if Ti 4+ was codoped with appropriate concentration. • The crystal field asymmetry was enhanced for better upconversion performance. • Crystal growth was prevented and small-sized NaYF 4 were obtained. - Abstract: 378 nm, 408 nm and 521 nm upconversion emissions of Er 3+ ions were obviously enhanced by Ti 4+ codoped with Yb 3+ /Er 3+ in hexagonal NaYF 4 , and the corresponding upconversion luminescence lifetimes were also prolonged, especially for 378 nm and 408 nm emissions. X-ray powder diffraction, field emission scanning electron microscope, transmission electron microscope, X-ray photoelectron spectroscopy and upconversion emission spectra were employed to explore the relationships of the structure and properties. From these characterizations we made a novel discovery that Na + could be induced to occupy Y 3+ sites for establishing valence balance of the system if Ti 4+ ions were codoped with appropriate concentration. As a result the crystal field asymmetry of NaY 0.92 Yb 0.05 Er 0.03 F 4 was enhanced and then its upconversion properties were improved because the hypersensitive electron transition of Yb 3+ /Er 3+ ions was promoted greatly. At the same time, the crystal sizes of the codoped NaYF 4 became smaller because the crystal growth was prevented by more negative charges gathering at the crystal surface. This study provides an exploration of the relationship among impurity doping, structural changes and upconversion performance, which may be useful for design and synthesis of high-performance upconversion codoping materials

Dielectric properties of layered FeGaInS{sub 4} single crystals in an alternating electric field

Energy Technology Data Exchange (ETDEWEB)

Mammadov, F. M. [Azerbaijan National Academy of Sciences, Nagiyev Institute of Catalysis and Inorganic Chemistry (Azerbaijan); Niftiyev, N. N., E-mail: namiq7@bk.ru [Azerbaijan State Pedagogical University (Azerbaijan)

2016-09-15

The results of investigations of the frequency and temperature dependences of dielectric losses and the imaginary part of the dielectric permittivity in FeGaInS{sub 4} single crystals are presented. Their experimental values are determined. It is established that the loss tangent and the imaginary part of the permittivity of FeGaInS{sub 4} single crystals in a field with frequencies of 10{sup 4}–10{sup 6} Hz decrease inversely proportional to the frequency (tanδ ~ 1/ω), and the conductivity is characterized by the band–hopping mechanism. For FeGaInS{sub 4}, the relaxation time is calculated, and it is established that there is a mechanism of electron polarization caused by thermal motion in this crystal.

X-ray detection capability of a Cs2ZnCl4 single-crystal scintillator

International Nuclear Information System (INIS)

Yahaba, Natsuna; Koshimizu, Masanori; Sun, Yan; Asai, Keisuke; Yanagida, Takayuki; Fujimoto, Yutaka; Haruki, Rie; Nishikido, Fumihiko; Kishimoto, Shunji

2014-01-01

The X-ray detection capability of a scintillation detector equipped with a Cs 2 ZnCl 4 single crystal was evaluated. The scintillation decay kinetics can be expressed as the sum of two exponential decay components. The fast decay component had a decay time constant of 1.8 ns, and its relative intensity was 95%. The total light output was 630 photons/MeV, and a subnanosecond timing resolution of 0.66 ns was obtained. The detection efficiency of 67.4 keV X-rays was 80% for a detector equipped with a 2.2-mm-thick Cs 2 ZnCl 4 crystal. Thus, excellent timing resolution and high detection efficiency were achieved simultaneously. (author)

Synchrotron white beam topography studies of SrLaGaO{sub 4} crystals

Energy Technology Data Exchange (ETDEWEB)

Wieteska, K. [Institute of Atomic Energy, 05-400 Otwock-Swierk (Poland); Wierzchowski, W. [Institute of Electronic Materials Technology, Wolczynska 133, 01-919 Warsaw (Poland)]. E-mail: wierzc_w@sp.itme.edu.pl; Graeff, W. [HASYLAB at DESY, Notkestr. 85, 22603 Hamburg (Germany); Lefeld-Sosnowska, M. [Institute of Experimental Physics, University of Warsaw, Hoza 69, 00-681 Warsaw (Poland); Pajaczkowska, A. [Institute of Electronic Materials Technology, Wolczynska 133, 01-919 Warsaw (Poland); Wierzbicka, E. [Institute of Electronic Materials Technology, Wolczynska 133, 01-919 Warsaw (Poland); Institute of Experimental Physics, University of Warsaw, Hoza 69, 00-681 Warsaw (Poland); Malinowska, A. [Institute of Experimental Physics, University of Warsaw, Hoza 69, 00-681 Warsaw (Poland); Faculty of Physics, Warsaw University of Technology, Koszykowa 75, 00-662 Warsaw (Poland); Institute of Electronic Materials Technology, Wolczynska 133, 01-919 Warsaw (Poland)

2005-09-29

Strontium lantanum gallate SrLaGaO{sub 4} tetragonal single crystal was investigated by white beam synchrotron radiation topography. Projection and section topographs were taken in back reflection and transmission geometry. The central 'core' crystal region was practically free of defects; only one extended 'oval' defect with strong boundary contrast was observed. The strong white-black contrasts connected with elongated volume defects and cracks were observed in surrounding the 'core' region.

Crystal structure and physical properties of CePt{sub 2.4}Al{sub 0.6}

Energy Technology Data Exchange (ETDEWEB)

Provino, A., E-mail: alessia.sting@gmail.com [Department of Chemistry, University of Genova, Via Dodecaneso 31, 16146 Genova (Italy); Institute SPIN-CNR, Corso Perrone 24, 16152 Genova (Italy); Bhattacharyya, A. [Department of Condensed Matter Physics and Materials Science, Tata Institute of Fundamental Research, Colaba, Mumbai 400005 (India); Science and Technology Facilities Council, Rutherford Appleton Laboratory, Excitations and Polarized Neutrons Group, Harwell Oxford, Didcot OX11 0QX (United Kingdom); Negretti, L. [Department of Chemistry, University of Genova, Via Dodecaneso 31, 16146 Genova (Italy); Kulkarni, R.; Thamizhavel, A.; Dhar, S.K. [Department of Condensed Matter Physics and Materials Science, Tata Institute of Fundamental Research, Colaba, Mumbai 400005 (India)

2015-02-15

Highlights: • New CePt{sub 2.4}Al{sub 0.6} compound crystallizes in the hexagonal CeNi{sub 3}-type (hP24, P6{sub 3}/mmc). • This crystal structure is a nearly ordered ternary derivative of CeNi{sub 3} prototype. • CePt{sub 2.4}Al{sub 0.6} compound orders ferromagnetically at 1.6 K; Ce ions in trivalent state. • Magnetization, electrical resistivity, low-T heat capacity have been measured. • Negative magnetoresistivity below ∼15 K shows short-range FM in paramagnetic state. - Abstract: The new compound CePt{sub 2.4}Al{sub 0.6} crystallizes in the hexagonal CeNi{sub 3}-type (hP24, space group P6{sub 3}/mmc, N. 194), with lattice parameters a = 5.5203(3) Å and c = 16.886(1) Å; its crystal structure represents a nearly ordered ternary derivative of this prototype. The cerium ions in CePt{sub 2.4}Al{sub 0.6} are in the normal trivalent state and order magnetically near 1.6 K as inferred from the low temperature heat capacity. The magnetic ordering is presumably ferromagnetic as suggested by the behavior of heat capacity in applied magnetic fields. The magnetoresistivity below ∼15 K is negative and is tentatively attributed to the presence of ferromagnetic short range order in the paramagnetic state.

Synthesis, spectra, and the crystal structure of α-(3,3-dimethyl-3,4-dihydroisoquinolyl-1)-hydroxyiminoacetamide

International Nuclear Information System (INIS)

Sokol, V.I.; Davydov, V.V.; Kartashova, I.V.; Zaitsev, B.E.; Shklyaev, Yu.V.; Ryabov, M.A.; Sergienko, V.S.

1996-01-01

α-(3,3-Dimethyl-3,4-dihydroisoquinolyl-1)-hydroxyiminoacetamide (I) was synthesized, and its x-ray structure analysis was performed (Enraf-Nonius CAD-4 diffractometer; MoKα radiation; graphite monochromator; θ/2θ scan; 2θmax=56 deg. ; 2496 reflections with I≥2σ(I); and R=0.038). Crystals of I are monoclinic; a=11.67(1), b=8.365(3), and c=15.22(2) A; β=107.7(1) deg.; V=1415.2(2) A 3; ρ(calc)=1.236 g/cm3; Z=4; and sp. gr. P21/n. I crystallizes as a monohydrate, and its formula is C13H15N3O2·H2O. In a crystal, I exists in a azomethineoxime tautomeric form. The planes of amideoxime and dihydroisoquinoline moieties are nearly orthogonal to each other. According to IR and electronic spectra, when passing from crystal to solution the conformation of I changes only slightly. An effect of water molecules on the molecular structure of I is discussed

Synthesis of Nanocrystalline CaWO4 as Low-Temperature Co-fired Ceramic Material: Processing, Structural and Physical Properties

Science.gov (United States)

Vidya, S.; Solomon, Sam; Thomas, J. K.

2013-01-01

Nanocrystalline scheelite CaWO4, a promising material for low-temperature co-fired ceramic (LTCC) applications, has been successfully synthesized through a single-step autoignition combustion route. Structural analysis of the sample was performed by powder x-ray diffraction (XRD), Fourier-transform infrared spectroscopy, and Raman spectroscopy. The XRD analysis revealed that the as-prepared sample was single phase with scheelite tetragonal structure. The basic optical properties and optical constants of the CaWO4 nanopowder were studied using ultraviolet (UV)-visible absorption spectroscopy, which showed that the material was a wide-bandgap semiconductor with bandgap of 4.7 eV at room temperature. The sample showed poor transmittance in the ultraviolet region but maximum transmission in the visible/near-infrared regions. The photoluminescence spectra recorded at different temperatures showed intense emission in the green region. The particle size estimated from transmission electron microscopy was 23 nm. The feasibility of CaWO4 for LTCC applications was studied from its sintering behavior. The sample was sintered at a relatively low temperature of 810°C to high density, without using any sintering aid. The surface morphology of the sintered sample was analyzed by scanning electron microscopy. The dielectric constant and loss factor of the sample measured at 5 MHz were found to be 10.50 and 1.56 × 10-3 at room temperature. The temperature coefficient of the dielectric constant was -88.71 ppm/°C. The experimental results obtained in this work demonstrate the potential of nano-CaWO4 as a low-temperature co-fired ceramic as well as an excellent luminescent material.

Pyroelectric Properties of Potassium and Rubidium Titanyl-Arsenate Single Crystals in the Temperature Range of 4.2-300 K

International Nuclear Information System (INIS)

Shaldin, Yu. V.; Matyjasik, S.; Novikova, N. E.; Tseitlin, M.; Mozhaev, E.; Roth, M.

2010-01-01

The temperature dependences of the pyroelectric coefficients of KTiOAsO 4 and RbTiOAsO 4 single crystals grown by flux crystallization have been investigated in the temperature range of 4.2-300 K. With an increase in temperature, superionic conductivity first arises in KTiOAsO4 (at T > 200 K) and then (at T > 270 K) in RbTiOAsO 4 . This conductivity is much higher in the samples polarized at T = 4.2 K. An exponential change in the crystal resistivity along the polar direction is simultaneously observed. The results of measurements in the range of 4.2-200 K indicate larger values of pyroelectric coefficients when compared with potassium and rubidium titanyl-phosphate crystals. A correlation between the pyroelectric coefficients and a change in the lattice constants at isomorphic substitutions of K atoms for Rb and P atoms for As has been revealed within the symmetry approach.

Pyroelectric Properties of Potassium and Rubidium Titanyl-Arsenate Single Crystals in the Temperature Range of 4.2-300 K

Energy Technology Data Exchange (ETDEWEB)

Shaldin, Yu. V., E-mail: yuri1999@rambler.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation); Matyjasik, S. [International Laboratory of Strong Magnetic Fields and Low Temperatures (Poland); Novikova, N. E. [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation); Tseitlin, M.; Mozhaev, E. [Ariel University Center of Samaria (Israel); Roth, M. [Hebrew University, School of Applied Sciences (Israel)

2010-11-15

The temperature dependences of the pyroelectric coefficients of KTiOAsO{sub 4} and RbTiOAsO{sub 4} single crystals grown by flux crystallization have been investigated in the temperature range of 4.2-300 K. With an increase in temperature, superionic conductivity first arises in KTiOAsO4 (at T > 200 K) and then (at T > 270 K) in RbTiOAsO{sub 4}. This conductivity is much higher in the samples polarized at T = 4.2 K. An exponential change in the crystal resistivity along the polar direction is simultaneously observed. The results of measurements in the range of 4.2-200 K indicate larger values of pyroelectric coefficients when compared with potassium and rubidium titanyl-phosphate crystals. A correlation between the pyroelectric coefficients and a change in the lattice constants at isomorphic substitutions of K atoms for Rb and P atoms for As has been revealed within the symmetry approach.

Crystal structure of [tris(4,4′-bipyridine]diium bis(1,1,3,3-tetracyano-2-ethoxypropenide trihydrate

Directory of Open Access Journals (Sweden)

Fatima Setifi

2016-09-01

Full Text Available The title hydrated salt, C30H26N62+·2C9H5N4O−·3H2O, was obtained as an unexpected product from the hydrothermal reaction between potassium 1,1,3,3-tetracyano-2-ethoxypropenide, 4,4′-bipyridine and iron(II sulfate heptahydrate. The cation lies across a twofold rotation axis in the space group I2/a with the other components all in general positions. In the cation, the H atom linking the pyridine units is disordered over two adjacent sites having occupancies of 0.66 (4 and 0.36 (4, i.e. as N—H...N and N...H—N. The water molecules of crystallization are each disordered over two sets of atomic sites, having occupancies of 0.522 (6 and 0.478 (6 for one, and 0.34 (3 and 0.16 (3 for the other, and it was not possible to reliably locate the H atoms associated with these partial-occupancy sites. In the crystal, four independent C—H...N hydrogen bonds link the ionic components into a three-dimensional network.

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

International Nuclear Information System (INIS)

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

2009-01-01

Ferroelastic β'-Gd 2 (MoO 4 ) 3 , (GMO), crystals are formed through the crystallization of 21.25Gd 2 O 3 -63.75MoO 3 -15B 2 O 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. - 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 β'-Gd 2 (MoO 4 ) 3 crystals are formed in the particle, and second harmonic generations are detected, depending on the domain structure.

Synthesis, crystal structure, electrical properties, and sodium transport pathways of the new arsenate Na{sub 4}Co{sub 7}(AsO{sub 4}){sub 6}

Energy Technology Data Exchange (ETDEWEB)

Ben Smida, Youssef; Marzouki, Riadh [Université de Tunis El Manar, Laboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Campus Universitaire, 2092 Manar II, Tunis (Tunisia); Georges, Samuel [Université Grenoble Alpes, Laboratoire d’Electrochimie et de Physicochimie des Matériaux et des Interfaces LEPMI, F-38000 Grenoble (France); Kutteh, Ramzi [Bragg Institute, Australian Nuclear Science and Technology Organisation (ANSTO), New Illawarra Road, Lucas Heights, New South Wales 2234 (Australia); Avdeev, Maxim [Bragg Institute, Australian Nuclear Science and Technology Organisation (ANSTO), New Illawarra Road, Lucas Heights, New South Wales 2234 (Australia); School of Chemistry, University of Sydney, Sydney, New South Wales 2006 (Australia); Guesmi, Abderrahmen; Zid, Mohamed Faouzi [Université de Tunis El Manar, Laboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Campus Universitaire, 2092 Manar II, Tunis (Tunisia)

2016-07-15

A new sodium cobalt (II) arsenate Na{sub 4}Co{sub 7}(AsO{sub 4}){sub 6} has been synthesized by a solid-state reaction and its crystal structure determined from single crystal X-ray diffraction data. It crystallizes in the monoclinic system, space group C2/m, with a=10.7098(9) Å, b=14.7837(9) Å, c=6.6845(7) Å, and β=105.545(9)°. The structure is described as a three-dimensional framework built up of corner-edge sharing CoO{sub 6}, CoO{sub 4} and AsO{sub 4} polyhedra, with interconnecting channels along [100] in which the Na{sup +} cations are located. The densest ceramics with relative density of 94% was obtained by ball milling and optimization of sintering temperature, and its microstructure characterized by scanning electron microscopy. The electrical properties of the ceramics were studied over a temperature interval from 280 °C to 560 °C using the complex impedance spectroscopy over the range of 13 MHz–5 Hz. The ionic bulk conductivity value of the sample at 360 °C is 2.51 10{sup −5} S cm{sup −1} and the measured activation energy is Ea=1 eV. The sodium migration pathways in the crystal structure were investigated computationally using the bond valence site energy (BVSE) model and classical molecular dynamics (MD) simulations. - Graphical abstract: Correlation between crystal structure, microstructure and ionic conductivity . Display Omitted - Highlights: • A new arsenate Na{sub 4}Co{sub 7}(AsO{sub 4}){sub 6} was prepared by solid state reaction. • Its crystal structure was determined by powder X-ray diffraction. • Na{sup +} ionic conductivity was probed by complex impedance spectroscopy. • Na{sup +} conduction pathways were modeled by bond-valence method and molecular dynamics.

Overexpression, crystallization and preliminary X-­ray crystallographic analysis of erythronate-4-phosphate dehydrogenase from Pseudomonas aeruginosa

Science.gov (United States)

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

The crystal structure of TeCl3+AuCl4-

International Nuclear Information System (INIS)

Jones, P.G.; Jentsch, D.; Schwarzmann, E.

1986-01-01

TeCl 3 + AuCl 4 - crystallizes in the triclinic space group Panti 1 with a=7.564(2), b=7.720(3), c=8.964(3) A, α=78.26(3), β=88.84(3), γ=89.35(3) 0 , Z=2. The structure was refined to R 0.041 for 1380 reflections. The cation polyhedron, including secondary Te...Cl interactions, is a square pyramid with mean Te-Cl 2.294, Te...Cl 3.028 A. The secondary interactions link the ions to form centrosymmetric (TeCl 3 .AuCl 4 ) 2 dimers. (orig.)

Crystallization kinetics of a-Se, part 4: thin films

Science.gov (United States)

Svoboda, Roman; Gutwirth, Jan; Málek, Jiří

2014-09-01

Differential scanning calorimetry was used to study the crystallization behaviour of selenium thin films in dependence on film thickness and deposition rate. In the current work, which is the fourth in a sequence of articles dealing with crystallization kinetics of a-Se, the non-isothermal crystallization kinetics was described in terms of the Johnson-Mehl-Avrami nucleation-growth model. Two-dimensional crystallite growth, consistent with the idea of sterically restricted crystallization in a thin layer, was confirmed for all data. It was found that neither the film thickness (tested within the 100-2350 nm range) nor the deposition rate appears to have any significant influence on the crystallization kinetics. However, the higher amount of intrinsic defects possibly produced by a higher deposition rate seems to accelerate the crystallization, shifting it towards lower temperatures. Very good correlation between the results obtained for thin films and those for fine powders was found. Based on the obtained results, interpretations of relevant literature data were made.

Spontaneous and stimulated emission in Sm3+-doped YAl3(BO3)4 single crystal

International Nuclear Information System (INIS)

Ryba-Romanowski, Witold; Lisiecki, Radosław; Beregi, Elena; Martín, I.R.

2015-01-01

Single crystals of YAl 3 (BO 3 ) 4 doped with trivalent samarium were grown by the top-seeded high temperature solution method and their absorption and emission spectra were investigated. Optical pumping into prominent absorption band around 405 nm feeds the 4 G 5/2 metastable level giving rise to intense visible luminescence distributed in several spectral lines with the most intense line around 600 nm characterized by a branching ratio of 0.42 and peak emission cross section of 0.25×10 −20 cm 2 . Optical amplification at 600 nm with a gain coefficient of 2.9 cm −1 was achieved during a pump-and-probe experiment. - Highlights: • YAB:Sm crystal grown by the top-seeded high temperature solution method. • Spectroscopic qualities relevant for visible laser operation. • YAB:Sm single crystal used in a pump-and-probe experiment. • Optical amplification properties of samarium doped YAl 3 (BO 3 ) 4

The oxidation of ReCl{sub 5} with oleum: synthesis and crystal structure of Re{sub 2}O{sub 4}Cl{sub 4}(SO{sub 4})

Energy Technology Data Exchange (ETDEWEB)

Betke, Ulf; Wickleder, Mathias S. [Carl von Ossietzky University of Oldenburg, Institute of Pure and Applied Chemistry (Germany)

2012-01-15

The reaction of ReCl{sub 5} and fuming sulfuric acid (25 % SO{sub 3}) in a sealed glass tube at 200 C led to red, needle shaped single crystals of Re{sub 2}O{sub 4}Cl{sub 4}(SO{sub 4}) (monoclinic, C2/c, a = 1501.8(2) pm, b = 1545.9(2) pm, c = 945.18(8) pm, β = 98.761(9) , Z = 8). In the crystal structure the [ReO{sub 2}] moieties are linked by [SO{sub 4}]{sup 2-} tetrahedra to chains along the [101] direction. Each sulfate ion connects four rhenium atoms, additional two chloride ions complete the octahedral coordination sphere of each rhenium atom according to {sup 1}{sub ∞}[ReO{sub 2/1}Cl{sub 2/1}(SO{sub 4}){sub 2/4}]. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

LASER APPLICATIONS AND OTHER TOPICS IN QUANTUM ELECTRONICS: Spectroscopy of V4+ and V3+ ions in a forsterite crystal

Science.gov (United States)

Veremeichik, T. F.; Gaister, A. V.; Zharikov, Evgeny V.; Protopopov, V. N.; Smirnov, Valerii A.; Subbotin, Kirill A.

2000-05-01

The absorption spectra of impurity vanadium ions in forsterite crystals are studied in the wavelength range from 600 to 2000 nm. It is found that the V4+ ion in the tetrahedral coordination in crystals grown by the Czochralski technique exhibits strong absorption in the range from 600 to 1200 nm. The intense electron-vibrational progressions in the absorption spectra of impurity d-ions in crystals were observed for the first time at temperatures 300 and 77 K. In the authors' opinion, these progressions appear due to the formation of the oxovanadate complex and distortions of the structural tetrahedron. The forsterite crystal doped with V4+ ions has a very high absorption cross section (up to 2.1×10-18 cm2) and a continuous broad absorption band, which makes this crystal promising as a passive laser switch in the range between 600 and 1200 nm. At the same time, the V4+ ions in the forsterite crystal do not emit luminescence because of a high probability of the nonradiative relaxation of their excited state. It is shown that luminescence of a V:Mg2SiO4 crystal is related to the tetrahedral V3+ ion.

Influence of MgSO{sub 4} doping on the properties of zinc tris–thiourea sulphate (ZTS) single crystals

Energy Technology Data Exchange (ETDEWEB)

Selvapandiyan, M., E-mail: mselvapandiyan@rediffmail.com [Department of Physics, Sri Vidya Mandir Arts and Science College, Uthangarai 635 207 (India); Arumugam, J. [Department of Physics, Sri Vidya Mandir Arts and Science College, Uthangarai 635 207 (India); Sundaramoorthi, P. [Department of Physics, Thiruvalluvar Government Arts College, Rasipuram 637 401 (India); Sudhakar, S. [CSIR–National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi 110 012 (India)

2013-12-15

Highlights: •The influence of MgSO{sub 4} doping on the properties of ZTS single crystals grown at room temperature. •Thermal stability of the crystals increased with incorporation of Mg atom. •Energy band gap was estimated from UV–vis spectra. •ZTS is a potential material for frequency conversion. •Both pure and doped ZTS crystals are belonging to category of typical insulating materials. -- Abstract: The influence of MgSO{sub 4} doping on the properties of zinc tris–thiourea sulphate single crystals grown at room temperature by slow evaporation solution growth technique was studied. Powder XRD analysis confirmed the orthorhombic crystal structure with noncentrosymmetric space group Pca2{sub 1}. The mechanical properties of the grown crystals were analysed by Vicker’s microhardness method. Functional groups present in the materials were identified by FTIR spectral analysis in the range between 4000 and 400 cm{sup −1}. The UV–Vis spectrum indicates that the UV cut-off wavelength of the crystals has less than 297 nm. The thermal stability of the grown crystals was determined with the aid of thermo-gravimetric analysis (TGA) and differential scanning calorimetry (DSC). Second order nonlinear optical behaviour of the grown crystals have been confirmed by Kurtz powder second harmonic generation (SHG) test.

High purity and semi-insulating 4H-SiC crystals grown by physical vapor transport

Energy Technology Data Exchange (ETDEWEB)

Augustine, G.; Hobgood, H.McD.; Balakrishna, V.; Dunne, G.T.; Hopkins, R.H.; Thomas, R.N. [Northrop Grumman Corp., Pittsburgh, PA (United States). Science and Technology Center; Doolittle, W.A.; Rohatgi, A. [Georgia Inst. of Tech., Atlanta, GA (United States). School of Electrical and Computer Engineering

1998-06-01

High purity undoped and semi-insulating vanadium doped 4H-SiC single crystals with diameters up to 50 mm were grown by the physical vapor transport method. Undoped crystals exhibiting resistivities in the 10{sup 2} to 10{sup 3} {Omega}-cm range and photoconductive decay (PCD) lifetimes in the 2 to 9 {mu}s range, were grown from high purity SiC sublimation sources. The crystals were p-type due to the presence of residual acceptor impurities, mainly boron. The semi-insulating behavior of the vanadium doped crystals is attributed to compensation of residual acceptors by the deep level vanadium donor located near the middle of the band gap. (orig.) 6 refs.

EXAFS investigations on PbMoO4 single crystals grown under ...

Indian Academy of Sciences (India)

Abstract. Extended X-ray absorption fine structure (EXAFS) measurements on PbMoO4 (LMO) crystals have been performed at the recently-commissioned dispersive EXAFS beamline (BL-8) of INDUS-2 Synchrotron facility at Indore, India. The LMO samples were prepared under three different conditions viz. (i) grown from ...

Crystal structure of 2-amino-4-(4-chlorophenyl-1-(4-methylphenyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carbonitrile

Directory of Open Access Journals (Sweden)

Shaaban K. Mohamed

2015-12-01

Full Text Available In the title compound, C23H20ClN3O, each of the cyclohexene and 1,4-dihydropyridine rings of the 1,4,5,6,7,8-hexahydroquinoline ring system adopts a twisted-boat conformation. The dihedral angle between the two benzene rings is 11.52 (7°. In the crystal, molecules are linked through a pair of amino–nitrile N—H...N hydrogen bonds, forming inversion dimers. These assemble into a three-dimensional network via C—H...O and C—H...π interactions.

Surface growth mechanisms and structural faulting in the growth of large single and spherulitic titanosilicate ETS-4 crystals

Science.gov (United States)

Miraglia, Peter Q.; Yilmaz, Bilge; Warzywoda, Juliusz; Sacco, Albert

2004-10-01

Morphological, surface and crystallographic analyses of titanosilicate ETS-4 products, with diverse habits ranging from spherulitic particles composed of submicron crystallites to large single crystals, are presented. Pole figures revealed that crystal surfaces with a-, b- and c- axes corresponded to , and directions, respectively. Thus, technologically important 8-membered ring pores and titania chains in ETS-4 run along the b-axis of single crystals and terminate at the smallest crystal face. Height of the spiral growth steps observed on {1 0 0} and {0 0 1} surfaces corresponded to the interplanar spacings associated with their crystallographic orientation, and is equivalent to the thickness of building units that form the ETS-4 framework. Data suggest that the more viscous synthesis mixtures, with a large driving force for growth, increased the two- and three-dimensional nucleation, while limiting the transport of nutrients to the growth surface. These conditions increase the tendency for stacking fault formation on {1 0 0} surfaces and small angle branching, which eventually results in spherulitic growth. The growth of high quality ETS-4 single crystals (from less viscous synthesis mixtures) occurred at lower surface nucleation rates. Data suggest that these high quality, large crystals grew due to one-dimensional nucleation at spiral hillocks, and indicate that under these conditions un-faulted growth is preferred.

Crystal structure of the alluaudite Ag{sub 2}Mn{sub 3}(VO{sub 4}){sub 3}

Energy Technology Data Exchange (ETDEWEB)

Yahia, Hamdi Ben; Essehli, Rachid; Belharouak, Ilias [Hamad Bin Khalifa Univ., Doha (Qatar). Qatar Environment and Energy Research Inst.; Shikano, Masahiro [National Institute of Advanced Industrial Science and Technology (AIST), Ikeda, Osaka (Japan). Research Inst. of Electrochemical Energy

2016-07-01

The new compound Ag{sub 2}Mn{sub 3}(VO4){sub 3} was synthesized by hydrothermal and solid state reaction routes, and its crystal structure was determined from single-crystal X-ray diffraction data. Ag{sub 2}Mn{sub 3}(VO4){sub 3} crystallizes with a monoclinic symmetry, space group C2/c, with a=11.8968(11) Aa, b=13.2057(13) Aa, c=6.8132(7) Aa, β=111.3166(15) ( ) and V=997.16(17) Aa{sup 3} (Z=4). Its crystal refinement yielded the residual factors R(F)=0.0249 and wR(F{sup 2})=0.0704 for 95 parameters and 1029 independent reflections at a 3σ(I) level. Ag{sub 2}Mn{sub 3}(VO4){sub 3} can be considered as a new member of the AA{sup '}MM{sup '}{sub 2}(XO4){sub 3} alluaudite family. The specific arrangement of M and M{sup '} octahedral sites and of X tetrahedral sites gives rise to two different channels aligned along the crystallographic c-axis and containing the A and A{sup '} sites. The A, A{sup '}, M, and X sites are fully occupied by Ag{sup +}, Mn{sup 2+}, and V{sup 5+}, respectively; whereas a Mn{sup 2+}/Mn{sup 3+} mixture is observed in the M{sup '} site.

The crystal structure of zwitterionic 2-{[(4-iminiumyl-3-methyl-1,4-dihydropyridin-1-ylmethyl]carbamoyl}benzoate hemihydrate

Directory of Open Access Journals (Sweden)

C. S. Chidan Kumar

2017-07-01

Full Text Available The asymmetric unit of the title compound, C15H15N3O3·0.5H2O, comprises two 2-{[(4-iminiumyl-3-methyl-1,4-dihydropyridin-1-ylmethyl]carbamoyl}benzoate zwitterions (A and B and a water molecule. The dihedral angles between the pyridine and phenyl rings in the zwitterions are 53.69 (10 and 73.56 (11° in A and B, respectively. In the crystal, molecules are linked by N—H...O, O—H...O, C—H...O and C—H...π(ring hydrogen bonds into a three-dimensional network. The crystal structure also features π–π interactions involving the centroids of the pyridine and phenyl rings [centroid–centroid distances = 3.5618 (12 Å in A and 3.8182 (14 Å in B].

Surface quality inspection of PbWO4 crystals by grazing incidence X-ray diffraction

International Nuclear Information System (INIS)

Mengucci, P.; Di Cristoforo, A.; Lebeau, M.; Majni, G.; Paone, N.; Pietroni, P.; Rinaldi, D.

2005-01-01

High-quality scintillating crystals are required for applications in radiographic systems and high-energy physics detectors to achieve the specified optical properties. In order to study the state of the single crystals surface we propose the use of the grazing incidence X-ray diffraction (GID) technique. This technique allows performing a depth profiling of the sample by changing the incidence angle of the X-ray beam with respect to the sample surface. In this work, two samples of a large PbWO 4 (PWO) single crystal exhibiting different surface roughness values have been studied. Results have shown that GID is a suitable technique for surface quality inspection

Synthesis and crystal structure of novel fluorescent 1,3,4-oxadiazole-containing carboxylate ligands

Science.gov (United States)

Mikhailov, Igor E.; Popov, Leonid D.; Tkachev, Valery V.; Aldoshin, Sergey M.; Dushenko, Galina A.; Revinskii, Yurii V.; Minkin, Vladimir I.

2018-04-01

Novel chelating ligands, 3-(5-aryl-1,3,4-oxadiazol-2-yl)acrylic acids and their zinc complexes were synthesized and their spectral and luminescent properties studied. The compounds intensively (quantum efficiencies φ = 0.18-0.76) luminesce in nonpolar solvents in the blue-green region (λmaxPL = 458-504 nm) of the spectrum. Molecular and crystal structures of 3-[5-(4-dimethylaminophenyl)-1,3,4-oxadiazol-2-yl]acrylic acid were established using X-ray crystallography. In crystal, the infinite chains of the molecules lie in the parallel planes and are arranged by the "head to tail" type to provide for strong π-π stacking interactions between the layers facilitating appearance of high electron transport properties and formation of excimers.

Purification, crystallization and preliminary X-ray crystallographic analysis of PBP4 from Listeria monocytogenes

International Nuclear Information System (INIS)

Jeong, Jae-Hee; Bae, Ji-Eun; Kim, Yeon-Gil

2011-01-01

The crystallization of PBP4 from L. monocytogenes is reported. Penicillin-binding proteins (PBPs), which catalyze peptidoglycan synthesis, have been extensively studied as a well established target of antimicrobial agents, including β-lactam derivatives. However, remarkable resistance to β-lactams has developed among pathogenic bacteria since the clinical use of penicillin began. Recently, the glycosyltransferase (GT) domain of class A PBPs has been proposed as an attractive target for antibiotic development as moenomycin-bound GT-domain structures have been determined. In this study, a class A PBP4 from Listeria monocytogenes was overexpressed, purified and crystallized using the hanging-drop vapour-diffusion method. Diffraction data were collected to 2.1 Å resolution using synchrotron radiation. The crystal belonged to the primitive orthorhombic space group P2 1 2 1 2, with unit-cell parameters a = 84.6, b = 127.8, c = 54.9 Å. The structural information will contribute to the further development of moenomycin-derived antibiotics possessing broad-spectrum activity

Overexpression, purification, crystallization and preliminary X-ray analysis of CheY4 from Vibrio cholerae O395

International Nuclear Information System (INIS)

Biswas, Maitree; Khamrui, Susmita; Sen, Udayaditya; Dasgupta, Jhimli

2011-01-01

The chemotaxis response regulator CheY4 from V. cholerae has been cloned, overexpressed, purified and crystallized in monoclinic and hexagonal space groups; the crystals diffracted to 1.67 and 1.9 Å resolution, respectively. Chemotaxis and motility greatly influence the infectivity of Vibrio cholerae, although the role of chemotaxis genes in V. cholerae pathogenesis is poorly understood. In contrast to the single copy of CheY found in Escherichia coli and Salmonella typhimurium, four CheYs (CheY1–CheY4) are present in V. cholerae. While insertional disruption of the cheY4 gene results in decreased motility, insertional duplication of this gene increases motility and causes enhanced expression of the two major virulence genes. Additionally, cheY3/cheY4 influences the activation of the transcription factor NF-κB, which triggers the generation of acute inflammatory responses. V. cholerae CheY4 was cloned, overexpressed and purified by Ni–NTA affinity chromatography followed by gel filtration. Crystals of CheY4 grown in space group C2 diffracted to 1.67 Å resolution, with unit-cell parameters a = 94.4, b = 31.9, c = 32.6 Å, β = 96.5°, whereas crystals grown in space group P3 2 21 diffracted to 1.9 Å resolution, with unit-cell parameters a = b = 56.104, c = 72.283 Å, γ = 120°

Al{sub 4}SiC{sub 4} wurtzite crystal: Structural, optoelectronic, elastic, and piezoelectric properties

Energy Technology Data Exchange (ETDEWEB)

Pedesseau, L., E-mail: laurent.pedesseau@insa-rennes.fr, E-mail: jacky.even@insa-rennes.fr; Even, J., E-mail: laurent.pedesseau@insa-rennes.fr, E-mail: jacky.even@insa-rennes.fr; Durand, O. [Fonctions Optiques pour les Technologies de l’Information, FOTON UMR 6082, CNRS, INSA de Rennes, 35708 Rennes (France); Modreanu, M. [Tyndall National Institute, University College Cork, Lee Maltings, Cork (Ireland); Chaussende, D.; Sarigiannidou, E.; Chaix-Pluchery, O. [LMGP, CNRS, Université Grenoble Alpes, 38000 Grenoble (France)

2015-12-01

New experimental results supported by theoretical analyses are proposed for aluminum silicon carbide (Al{sub 4}SiC{sub 4}). A state of the art implementation of the density functional theory is used to analyze the experimental crystal structure, the Born charges, the elastic properties, and the piezoelectric properties. The Born charge tensor is correlated to the local bonding environment for each atom. The electronic band structure is computed including self-consistent many-body corrections. Al{sub 4}SiC{sub 4} material properties are compared to other wide band gap wurtzite materials. From a comparison between an ellipsometry study of the optical properties and theoretical results, we conclude that the Al{sub 4}SiC{sub 4} material has indirect and direct band gap energies of about 2.5 eV and 3.2 eV, respectively.

Non-Covalent Interactions in the Crystal Structure of Methyl 4-Hydroxy-3-Nitrobenzoate

Directory of Open Access Journals (Sweden)

Jim Simpson

2012-06-01

Full Text Available Methyl 4-hydroxy-3-nitrobenzoate, (I, C8H7NO5, crystallizes with two unique molecules, A and B, in the asymmetric unit of the triclinic unit cell. The space group was assigned as P-1, with lattice parameters a = 0.72831(15, b = 1.0522(2, c = 1.1410(2 nm, α = 83.38(3, β = 80.83(3, γ = 82.02(3°, Z = 4, V = 0.8510(3 nm3, Mr = 197.15, Dc = 1.539 g/m3, µ= 0.131 mm−1, F(000 = 408, R = 0.1002 and wR = 0.2519. In the crystal structure, 12 hydrogen bonding and two p-stacking interactions link the molecules into infinite stacked sheets parallel to (101.

Crystal structure of 4,4′-bis[3-(piperidin-1-ylprop-1-yn-1-yl]-1,1′-biphenyl

Directory of Open Access Journals (Sweden)

Anqi Walbaum

2017-06-01

Full Text Available The title compound, C28H32N2, (I, is one of a second generation of compounds designed and synthesized based on a very potent and selective α9α10 nicotinic acetylcholine receptor antagonist ZZ161C {1,1′-[[1,1′-biphenyl]-4,4′-diylbis(prop-2-yne-3,1-diyl]bis(3,4-dimethylpyridin-1-ium bromide}, which has shown analgesic effects in a chemotherapy-induced neuropathy animal model. Compound (I was synthesized by the reaction of 4,4′-bis(3-bromoprop-1-yn-1-yl-1,1′-biphenyl with piperidine at room temperature in acetonitrile. The single-crystal used for X-ray analysis was obtained by dissolving (I in a mixture of dichloromethane and methanol, followed by slow evaporation of the solvent. In the crystal of (I, the biphenyl moiety has a twisted conformation, with a dihedral angle of 25.93 (4° between the benzene rings. Both piperidine head groups in (I are in the chair conformation and are oriented so that the N-atom lone pairs of each piperidine group point away from the central biphenyl moiety.

Crystal structures of p-substituted derivatives of 2,6-dimethylbromobenzene with ½ ≤ Z′ ≤ 4

Directory of Open Access Journals (Sweden)

Angélica Navarrete Guitérrez

2016-12-01

Full Text Available The crystal structures of four bromoarenes based on 2,6-dimethylbromobenzene are reported, which are differentiated according the functional group X placed para to the Br atom: X = CN (4-bromo-3,5-dimethylbenzonitrile, C9H8BrN, (1, X = NO2 (2-bromo-1,3-dimethyl-5-nitrobenzene, C8H8BrNO2, (2, X = NH2 (4-bromo-3,5-dimethylaniline, C8H10BrN, (3 and X = OH (4-bromo-3,5-dimethylphenol, C8H9BrO, (4. The content of the asymmetric unit is different in each crystal, Z′ = ½ (X = CN, Z′ = 1 (X = NO2, Z′ = 2 (X = NH2, and Z′ = 4 (X = OH, and is related to the molecular symmetry and the propensity of X to be involved in hydrogen bonding. In none of the studied compounds does the crystal structure feature other non-covalent interactions, such as π–π, C—H...π or C—Br...Br contacts.

Slow neutron scattering in molecular crystals. 5-4

International Nuclear Information System (INIS)

Inoue, Kazuhiko

1976-01-01

The utilization of incoherent inelastic neutron scattering (INS) as a probe for molecular crystals is reviewed. In particular, some typical examples of the measurement of incoherent inelastic neutron scattering spectra (INSS) in molecular crystals are presented in the first section of this report. The results of measurement are shown for theta-xylene, benzene, polypropylene oxide, deuteride, and formic acid. The second section presents an equation for the incoherent scattering cross section of a crystal by dividing the molecular motion into the outer and inner modes. Phonon expansion is also used for the easy understanding of the relation between the INSS and the dynamic characteristics of molecular crystals. In the third section, the measured results are analyzed on the basis of the theory presented in the previous section. And the difference between the van der Waals bond and the hydrogen bond is shortly discussed. (Aoki, K.)

Si{sub 3}N{sub 4} optomechanical crystals in the resolved-sideband regime

Energy Technology Data Exchange (ETDEWEB)

Davanço, M., E-mail: mdavanco@nist.gov [Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, Maryland 20899 (United States); Department of Applied Physics, California Institute of Technology, Pasadena, California 91125 (United States); Ates, S.; Liu, Y. [Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, Maryland 20899 (United States); Maryland NanoCenter, University of Maryland, College Park, Maryland 20742 (United States); Srinivasan, K. [Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, Maryland 20899 (United States)

2014-01-27

We demonstrate sideband-resolved Si{sub 3}N{sub 4} optomechanical crystals supporting 10{sup 5} quality factor optical modes at 980 nm, coupled to ≈4 GHz frequency mechanical modes with quality factors of ≈3000. Optomechanical electromagnetically induced transparency and absorption are observed at room temperature and in atmosphere with intracavity photon numbers in excess of 10{sup 4}.

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

Science.gov (United States)

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.

Influence of Nd dopants on lattice parameters and thermal and elastic properties in YVO4 single crystals

International Nuclear Information System (INIS)

Kucytowski, J.; Wokulska, K.; Kazmierczak-Balata, A.; Bodzenta, J.; Lukasiewicz, T.; Hofman, B.; Pyka, M.

2008-01-01

The influence of neodymium doping on YVO 4 single crystals has been studied. The crystals were grown by the Czochralski method. One of them was pure YVO 4 and the others were doped with neodymium (YVO 4 :Nd) at various concentrations of Nd = 0.3-3.0 at.%. The changes of the lattice parameters were determined by the Bond's method [W.L. Bond, Acta Cryst. 13 (1960) 814]. The thermal diffusivity and the velocity of ultrasound using the photothermal method with mirage effect and the pulse echo method [J. Bodzenta, M. Pyka, J. Phys. IV France 137 (2006) 259] were measured. In the examined crystals, it was found that the lattice parameters increase while the thermal diffusivity decreases with increasing concentration of Nd atoms

High-pressure crystal growth and magnetic and electrical properties of the quasi-one dimensional osmium oxide Na2OsO4

International Nuclear Information System (INIS)

Shi, Y.G.; Guo, Y.F.; Yu, S.; Arai, M.; Belik, A.A.; Sato, A.; Yamaura, K.; Takayama-Muromachi, E.

2010-01-01

Na 2 OsO 4 crystals were grown by a NaCl flux method under high pressure. It crystallizes in the Ca 2 IrO 4 -type structure without having additional elements or metal vacancies, which are usually accommodated. It appears that Na 2 OsO 4 is a metal-stoichiometric Ca 2 IrO 4 -type compound never been synthesized to date. Na 2 OsO 4 has the octahedral environment of Os 6+ O 6 so that the electronic configuration is 5d 2 , suggesting the magnetic S=1 ground state. However, magnetization, electrical resistivity, and specific heat measurements indicated that the non-magnetic S=0 state is much likely for Na 2 OsO 4 than the S=1 state. Band structure calculations and the structure analysis found that the disagreement is probably due to the statically uniaxial compression of the OsO 6 octahedra, resulting in splitting of the t 2 g band. - Graphical abstract: Na 2 OsO 4 crystals were grown by a NaCl flux method under high pressure. It crystallizes in the Ca 2 IrO 4 -type structure comprising infinite Os 6+ O 6 octahedra (5d 2 ) chains. The crystal growth, the crystal structure, and the magnetic and electrical properties are reported.

Molecular and crystal structure of 2-((E)-[(4-Methylphenyl)imino]methyl)-4-nitrophenol: A redetermination

Energy Technology Data Exchange (ETDEWEB)

Kaynar, Nihal Kan, E-mail: nihal-kan84@windowslive.com [Ondokuz Mayıs University, Department of Physics, Faculty of Arts and Sciences (Turkey); Tanak, Hasan [Amasya University, Department of Physics, Faculty of Arts and Sciences (Turkey); Şahin, Songul [Ondokuz Mayıs University, Department of Chemistry, Faculty of Arts and Sciences (Turkey); Dege, Necmi [Ondokuz Mayıs University, Department of Physics, Faculty of Arts and Sciences (Turkey); Ağar, Erbil [Ondokuz Mayıs University, Department of Chemistry, Faculty of Arts and Sciences (Turkey); Yavuz, Metin [Ondokuz Mayıs University, Department of Physics, Faculty of Arts and Sciences (Turkey)

2016-03-15

The crystal structure of the title compound, C{sub 14}H{sub 12}N{sub 2}O{sub 3}, was recently determined as a mixture of its neutral (OH containing) and zwitterionic (NH containing) forms, in a 0.60 (4): 0.40 (4) ratio using the X-ray determination. In this study, the title compound has been characterized by FT-IR and X-ray diffraction. The redetermination showed that the title compound has only enol (OH) form because of lack of the NH stretching vibration in FT-IR spectrum. In addition, the molecular structure and tautomerism of the title compound have been discussed.

Optical sensor platform based on cellulose nanocrystals (CNC) - 4'-(hexyloxy)-4-biphenylcarbonitrile (HOBC) bi-phase nematic liquid crystal composite films.

Science.gov (United States)