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Sample records for sample crystal shows

  1. Synchrotron/crystal sample preparation

    Science.gov (United States)

    Johnson, R. Barry

    1993-01-01

    The Center for Applied Optics (CAO) of the University of Alabama in Huntsville (UAH) prepared this final report entitled 'Synchrotron/Crystal Sample Preparation' in completion of contract NAS8-38609, Delivery Order No. 53. Hughes Danbury Optical Systems (HDOS) is manufacturing the Advanced X-ray Astrophysics Facility (AXAF) mirrors. These thin-walled, grazing incidence, Wolter Type-1 mirrors, varying in diameter from 1.2 to 0.68 meters, must be ground and polished using state-of-the-art techniques in order to prevent undue stress due to damage or the presence of crystals and inclusions. The effect of crystals on the polishing and grinding process must also be understood. This involves coating special samples of Zerodur and measuring the reflectivity of the coatings in a synchrotron system. In order to gain the understanding needed on the effect of the Zerodur crystals by the grinding and polishing process, UAH prepared glass samples by cutting, grinding, etching, and polishing as required to meet specifications for witness bars for synchrotron measurements and for investigations of crystals embedded in Zerodur. UAH then characterized these samples for subsurface damage and surface roughness and figure.

  2. Sample Size Induced Brittle-to-Ductile Transition of Single-Crystal Aluminum Nitride

    Science.gov (United States)

    2015-08-01

    ARL-RP-0528 ● AUG 2015 US Army Research Laboratory Sample Size Induced Brittle-to- Ductile Transition of Single-Crystal Aluminum...originator. ARL-RP-0528 ● AUG 2015 US Army Research Laboratory Sample Size Induced Brittle-to- Ductile Transition of Single-Crystal...Sample Size Induced Brittle-to- Ductile Transition of Single-Crystal Aluminum Nitride 5a. CONTRACT NUMBER 5b. GRANT NUMBER 5c. PROGRAM ELEMENT

  3. The influence of freezer storage of urine samples on the BONN-Risk-Index for calcium oxalate crystallization.

    Science.gov (United States)

    Laube, Norbert; Zimmermann, Diana J

    2004-01-01

    This study was performed to quantify the effect of a 1-week freezer storage of urine on its calcium oxalate crystallization risk. Calcium oxalate is the most common urinary stone material observed in urolithiasis patients in western and affluent countries. The BONN-Risk-Index of calcium oxalate crystallization risk in human urine is determined from a crystallization experiment performed on untreated native urine samples. We tested the influence of a 1-week freezing on the BONN-Risk-Index value as well as the effect of the sample freezing on the urinary osmolality. In vitro crystallization experiments in 49 native urine samples from stone-forming and non-stone forming individuals were performed in order to determine their calcium oxalate crystallization risk according to the BONN-Risk-Index approach. Comparison of the results derived from original sample investigations with those obtained from the thawed aliquots by statistical evaluation shows that i) no significant deviation from linearity between both results exists and ii) both results are identical by statistical means. This is valid for both, the BONN-Risk-Index and the osmolality data. The differences in the BONN-Risk-Index results of both procedures of BONN-Risk-Index determination, however, exceed the clinically acceptable difference. Thus, determination of the urinary calcium oxalate crystallization risk from thawed urine samples cannot be recommended.

  4. Pi sampling: a methodical and flexible approach to initial macromolecular crystallization screening

    International Nuclear Information System (INIS)

    Gorrec, Fabrice; Palmer, Colin M.; Lebon, Guillaume; Warne, Tony

    2011-01-01

    Pi sampling, derived from the incomplete factorial approach, is an effort to maximize the diversity of macromolecular crystallization conditions and to facilitate the preparation of 96-condition initial screens. The Pi sampling method is derived from the incomplete factorial approach to macromolecular crystallization screen design. The resulting ‘Pi screens’ have a modular distribution of a given set of up to 36 stock solutions. Maximally diverse conditions can be produced by taking into account the properties of the chemicals used in the formulation and the concentrations of the corresponding solutions. The Pi sampling method has been implemented in a web-based application that generates screen formulations and recipes. It is particularly adapted to screens consisting of 96 different conditions. The flexibility and efficiency of Pi sampling is demonstrated by the crystallization of soluble proteins and of an integral membrane-protein sample

  5. A low-temperature sample orienting device for single crystal spectroscopy at the SNS

    Energy Technology Data Exchange (ETDEWEB)

    Sherline, T E; Solomon, L; Roberts, C K II; Bruce, D; Gaulin, B; Granroth, G E, E-mail: sherlinete@ornl.gov

    2010-11-01

    A low temperature sample orientation device providing three axes of rotation has been successfully built and is in testing for use on several spectrometers at the spallation neutron source (SNS). Sample rotation about the vertical ({omega}) axis of nearly 360 deg. and out of plane tilts ({phi} and v) of from -3.4 deg. to 4.4 deg. and from -2.8 deg. to 3.5 deg., respectively, are possible. An off-the-shelf closed cycle refrigerator (CCR) is mounted on a room temperature sealed rotary flange providing {omega} rotations of the sample. Out-of-plane tilts are made possible by piezoelectric actuated angular positioning devices mounted on the low temperature head of the CCR. Novel encoding devices based on magnetoresistive sensors have been developed to measure the tilt stage angles. This combination facilitates single crystal investigations from room temperature to 3.1 K. Commissioning experiments of the rotating CCR for both powder and single crystal samples have been performed on the ARCS spectrometer at the SNS. For the powder sample this device was used to continuously rotate the sample and thus average out any partial orientation of the powder. The powder rings observed in S(Q) are presented. For the single crystal sample, the rotation was used to probe different regions of momentum transfer (Q-space). Laue patterns obtained from a single crystal sample at two rotation angles are presented.

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

    Energy Technology Data Exchange (ETDEWEB)

    Pan, Bo; Shibutani, Yoji, E-mail: sibutani@mech.eng.osaka-u.ac.jp [Department of Mechanical Engineering, Osaka University, Suita 565-0871 (Japan); Zhang, Xu [State Key Laboratory for Strength and Vibration of Mechanical Structures, School of Aerospace, Xi' an Jiaotong University, Xi' an 710049 (China); School of Mechanics and Engineering Science, Zhengzhou University, Zhengzhou 450001 (China); Shang, Fulin [State Key Laboratory for Strength and Vibration of Mechanical Structures, School of Aerospace, Xi' an Jiaotong University, Xi' an 710049 (China)

    2015-07-07

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

  7. Highly oriented Bi-system bulk sample prepared by a decomposition-crystallization process

    International Nuclear Information System (INIS)

    Xi Zhengping; Zhou Lian; Ji Chunlin

    1992-01-01

    A decomposition-crystallization method, preparing highly oriented Bi-system bulk sample is reported. The effects of processing parameter, decomposition temperature, cooling rate and post-treatment condition on texture and superconductivity are investigated. The method has successfully prepared highly textured Bi-system bulk samples. High temperature annealing does not destroy the growing texture, but the cooling rate has some effect on texture and superconductivity. Annealing in N 2 /O 2 atmosphere can improve superconductivity of the textured sample. The study on the superconductivity of the Bi(Pb)-Sr-Ca-Cu-O bulk material has been reported in numerous papers. The research on J c concentrates on the tape containing the 2223 phase, with very few studies on the J c of bulk sample. The reason for the lack of studies is that the change of superconducting phases at high temperatures has not been known. The authors have reported that the 2212 phase incongruently melted at about 875 degrees C and proceeded to orient the c-axis perpendicular to the surface in the process of crystallization of the 2212 phase. Based on that result, a decomposition-crystallization method was proposed to prepare highly oriented Bi-system bulk sample. In this paper, the process is described in detail and the effects of processing parameters on texture and superconductivity are reported

  8. Stepwise crystallization and the layered distribution in crystallization kinetics of ultra-thin poly(ethylene terephthalate) film

    Energy Technology Data Exchange (ETDEWEB)

    Zuo, Biao, E-mail: chemizuo@zstu.edu.cn, E-mail: wxinping@yahoo.com; Xu, Jianquan; Sun, Shuzheng; Liu, Yue; Yang, Juping; Zhang, Li; Wang, Xinping, E-mail: chemizuo@zstu.edu.cn, E-mail: wxinping@yahoo.com [Department of Chemistry, Key Laboratory of Advanced Textile Materials and Manufacturing Technology of the Education Ministry, Zhejiang Sci-Tech University, Hangzhou 310018 (China)

    2016-06-21

    Crystallization is an important property of polymeric materials. In conventional viewpoint, the transformation of disordered chains into crystals is usually a spatially homogeneous process (i.e., it occurs simultaneously throughout the sample), that is, the crystallization rate at each local position within the sample is almost the same. Here, we show that crystallization of ultra-thin poly(ethylene terephthalate) (PET) films can occur in the heterogeneous way, exhibiting a stepwise crystallization process. We found that the layered distribution of glass transition dynamics of thin film modifies the corresponding crystallization behavior, giving rise to the layered distribution of the crystallization kinetics of PET films, with an 11-nm-thick surface layer having faster crystallization rate and the underlying layer showing bulk-like behavior. The layered distribution in crystallization kinetics results in a particular stepwise crystallization behavior during heating the sample, with the two cold-crystallization temperatures separated by up to 20 K. Meanwhile, interfacial interaction is crucial for the occurrence of the heterogeneous crystallization, as the thin film crystallizes simultaneously if the interfacial interaction is relatively strong. We anticipate that this mechanism of stepwise crystallization of thin polymeric films will allow new insight into the chain organization in confined environments and permit independent manipulation of localized properties of nanomaterials.

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

    Science.gov (United States)

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

    2003-01-15

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

  10. Stability of equilibrium states in finite samples of smectic C* liquid crystals

    International Nuclear Information System (INIS)

    Stewart, I W

    2005-01-01

    Equilibrium solutions for a sample of ferroelectric smectic C (SmC*) liquid crystal in the 'bookshelf' geometry under the influence of a tilted electric field will be presented. A linear stability criterion is identified and used to confirm stability for typical materials possessing either positive or negative dielectric anisotropy. The theoretical response times for perturbations to the equilibrium solutions are calculated numerically and found to be consistent with estimates for response times in ferroelectric smectic C liquid crystals reported elsewhere in the literature for non-tilted fields

  11. Stability of equilibrium states in finite samples of smectic C* liquid crystals

    Energy Technology Data Exchange (ETDEWEB)

    Stewart, I W [Department of Mathematics, University of Strathclyde, Livingstone Tower, 26 Richmond Street, Glasgow G1 1XH (United Kingdom)

    2005-03-04

    Equilibrium solutions for a sample of ferroelectric smectic C (SmC*) liquid crystal in the 'bookshelf' geometry under the influence of a tilted electric field will be presented. A linear stability criterion is identified and used to confirm stability for typical materials possessing either positive or negative dielectric anisotropy. The theoretical response times for perturbations to the equilibrium solutions are calculated numerically and found to be consistent with estimates for response times in ferroelectric smectic C liquid crystals reported elsewhere in the literature for non-tilted fields.

  12. Payload specialist Reinhard Furrer show evidence of previous blood sampling

    Science.gov (United States)

    1985-01-01

    Payload specialist Reinhard Furrer shows evidence of previous blood sampling while Wubbo J. Ockels, Dutch payload specialist (only partially visible), extends his right arm after a sample has been taken. Both men show bruises on their arms.

  13. An FPGA-based sampling-ADC readout for the crystal barrel calorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Muellers, Johannes [Helmholtz-Institut fuer Strahlen- und Kernphysik, Bonn (Germany); Marciniewski, Pawel [Angstroemlaboratoriet, Uppsala (Sweden); Collaboration: CBELSA/TAPS-Collaboration

    2015-07-01

    The CBELSA/TAPS experiment at the electron accelerator ELSA (Bonn) investigates the photoproduction of mesons off protons and neutrons. Presently the readout of the CsI(Tl)-crystals of the Crystal Barrel calorimeter is being upgraded from a PIN-diode readout to an APD readout to create a fast signal for first-level-triggering. This will increase the trigger efficiency especially for final states with only neutral particles substantially. To increase the possible data readout rate, which is currently limited by the digitization stage (LeCroy QDC 1885F) to ∼ 2 kHz, the implementation of a new Sampling-ADC (SADC) readout is being prepared. Based on the 64-channel PANDA-SADC, the CB-SADC design was modified and adapted to the needs of the CBELSA/TAPS experiment. It offers 64 channels in one NIM module, together with modular analog or FPGA-based digital shaping. The data transfer will be realized by two standard gigabit links. Using an FPGA together with SADCs provides a multitude of possibilities for online feature extraction, such as the determination of the energy deposited in the crystal, TDC capabilities and pile-up detection and recovery.

  14. Observations related to hydrogen in powder and single crystal samples of YB2Cu3O7-δ

    International Nuclear Information System (INIS)

    Porath, D.; Grayevsky, A.; Kaplan, N.; Shaltiel, D.; Yaron, U.; Walker, E.

    1994-01-01

    New observations related to hydrogenation of YBa 2 Cu 3 O 7-δ (YBCO) are reported: (a) The effects of sample preparation on the H concentration in ''uncharged'' YBCO samples is investigated, and it is shown through nuclear magnetic resonance measurements that samples of YBCO prepared by ''standard'' solid-state reaction procedures may contain ab initio up to 0.2 atoms formula -1 of hydrogen. (b) It is demonstrated that one may introduce up to 0.3 atoms formula -1 into single crystal samples of YBCO without destroying the macroscopic crystal. The significance of the above observations is discussed briefly. (orig.)

  15. Compensation Methods for Non-uniform and Incomplete Data Sampling in High Resolution PET with Multiple Scintillation Crystal Layers

    International Nuclear Information System (INIS)

    Lee, Jae Sung; Kim, Soo Mee; Lee, Dong Soo; Hong, Jong Hong; Sim, Kwang Souk; Rhee, June Tak

    2008-01-01

    To establish the methods for sinogram formation and correction in order to appropriately apply the filtered backprojection (FBP) reconstruction algorithm to the data acquired using PET scanner with multiple scintillation crystal layers. Formation for raw PET data storage and conversion methods from listmode data to histogram and sinogram were optimized. To solve the various problems occurred while the raw histogram was converted into sinogram, optimal sampling strategy and sampling efficiency correction method were investigated. Gap compensation methods that is unique in this system were also investigated. All the sinogram data were reconstructed using 2D filtered backprojection algorithm and compared to estimate the improvements by the correction algorithms. Optimal radial sampling interval and number of angular samples in terms of the sampling theorem and sampling efficiency correction algorithm were pitch/2 and 120, respectively. By applying the sampling efficiency correction and gap compensation, artifacts and background noise on the reconstructed image could be reduced. Conversion method from the histogram to sinogram was investigated for the FBP reconstruction of data acquired using multiple scintillation crystal layers. This method will be useful for the fast 2D reconstruction of multiple crystal layer PET data

  16. Crystal orientation and sample preparation effects on sputtering and lattice damage in 100 keV self-irradiated copper

    International Nuclear Information System (INIS)

    Sprague, J.A.; Malmberg, P.R.; Reynolds, G.W.; Lambert, J.M.; Treado, P.A.; Vincenz, A.M.

    1987-01-01

    Sputtering yields and angular distributions have been measured as functions of sample preparation techniques and incident ion-beam orientation with respect to the crystal axes for 100 keV Cu-ion beams on Cu crystals and polycrystalline samples. The angular distributions have structure requiring an nth order cosine with two Gaussians superimposed to fit the data; strong peaking is observed near the backscatter direction. The yield is dependent on the beam to crystal and beam to polycrystalline-rod axis orientation, on the grain size of the polycrystals and on sample-preparation techniques. Yield measurements vary by as much as a factor of 4. Lattice-damage differences, measured with alpha particle channeling, are much smaller and seem to be saturated by fluences of the order of 1x10 16 /cm 2 . (orig.)

  17. Molecular Weight and Crystallization Temperature Effects on Poly(ethylene terephthalate (PET Homopolymers, an Isothermal Crystallization Analysis

    Directory of Open Access Journals (Sweden)

    Leonardo A. Baldenegro-Perez

    2014-02-01

    Full Text Available The isothermal crystallization of poly(ethylene terephthalate (PET homopolymers with different molecular weight was studied in a wide temperature range (140–230 °C using different experimental techniques. Three different morphological regions, labeled r1, r2 and r3, were distinguished as a function of crystallization temperature (Tc. In r1 (low Tc crystallized samples were characterized by a low crystalline degree with a small spherulite texture containing thin crystals. In r2 (intermediate Tc samples showed medium size spherulites composed of two distinct crystalline families (thin and thick crystals. In this temperature range, the crystallization exhibited a maximum value and it was associated with a high content of secondary crystals. In r3 (high Tc, samples presented considerable amorphous zones and regions consisting of oversized spherulites containing only thick crystals. Time-resolved wide-angle X-ray diffraction measurements, using synchrotron radiation, indicated a rapid evolution of the crystalline degree within the second region, in contrast with the quite slow evolution observed in the third region. On the other hand, by small-angle X-ray scattering (SAXS and time-resolved SAXS experiment, it was found that the long period (L as well as the lamellar thickness (lc increase as a function of Tc, corroborating the formation of the thickest crystals in the third region. From all these observations, a morphological model was proposed for each region.

  18. Crystallization characteristics of iron-rich glass ceramics prepared from nickel slag and blast furnace slag

    Science.gov (United States)

    Wang, Zhong-Jie; Ni, Wen; Li, Ke-Qing; Huang, Xiao-Yan; Zhu, Li-Ping

    2011-08-01

    The crystallization process of iron-rich glass-ceramics prepared from the mixture of nickel slag (NS) and blast furnace slag (BFS) with a small amount of quartz sand was investigated. A modified melting method which was more energy-saving than the traditional methods was used to control the crystallization process. The results show that the iron-rich system has much lower melting temperature, glass transition temperature ( T g), and glass crystallization temperature ( T c), which can result in a further energy-saving process. The results also show that the system has a quick but controllable crystallization process with its peak crystallization temperature at 918°C. The crystallization of augite crystals begins from the edge of the sample and invades into the whole sample. The crystallization process can be completed in a few minutes. A distinct boundary between the crystallized part and the non-crystallized part exists during the process. In the non-crystallized part showing a black colour, some sphere-shaped augite crystals already exist in the glass matrix before samples are heated to T c. In the crystallized part showing a khaki colour, a compact structure is formed by augite crystals.

  19. Physico-mechanical and dissolution behaviours of ibuprofen crystals crystallized in the presence of various additives

    Directory of Open Access Journals (Sweden)

    A Nokhodchi

    2010-06-01

    Full Text Available "n  "n Background and the purpose of the study: The success of any direct-tableting procedure is strongly affected by the quality of the crystals used in the process. Ibuprofen is a poorly compactible drug with a high tendency for capping. In order to use ibuprofen in direct compression formulations, physico-mechanical properties of ibuprofen should be improved considerably. The aim of the present investigation was to employ crystallization techniques in order to improve the physico-mechanical properties of ibuprofen for direct compression. "nMethods:The experimental methods involved the preparation of ibuprofen crystals by solvent change technique. Ibuprofen was dissolved in ethanol and crystallized out with water in the absence or presence of various hydrophilic additives (PEG 6000, 8000, Brij 98P and polyvinyl alcohol 22000, PVA 22000 with different concentrations. The physico-mechanical properties of the ibuprofen crystals were studied in terms of flow, density, tensile strength and dissolution behaviour. Morphology of ibuprofen crystals was studied by scanning electron microscopic (SEM. Solid state of the recrystallized particles was also investigated using differential scanning calorimeter (DSC and FT-IR. "nResults:Ibuprofen samples crystallized in the presence of PEG 6000 and 8000 and PVA showed remarkable increase in the tensile strengths of the directly compressed tablets, while some other additives, i.e. Brij 98P did not produce improved ibuprofen crystals. Ibuprofen powders made from particles obtained in the presence of PVA and Brij 98P showed similar dissolution profiles to the commercial ibuprofen particles. DSC and FT-IR results ruled out any significant interaction between ibuprofen and additives except for the samples crystallized in the presence of PEG 8000. Conclusion:The crystal habit of ibuprofen can be altered successfully by the crystallization technique which was developed in this study. The crystals developed in the

  20. Cultivation and characterization of GaInSe2 crystals

    International Nuclear Information System (INIS)

    Panakhov, T.M.; Kafarova, D.M.

    2013-01-01

    This work is the first systematic study devoted to the growth of GaInSe 2 crystals and their characterization by experimental methods such as X-ray diffraction, electron microscopy transmission with high resolution, sample electron diffraction. By the method of photoelectron roentgen spectroscopy it was studied the chemical structure of the GaInSe 2 crystals and the microprobe analysis indicated that the individual crystals have an excess of gallium. GaInSe 2 crystals were grown by the Bridgman method. Samples were prepared as single crystals by the Bridgman method. Studies showed that the GaInSe 2 crystals are hexagonal ones

  1. Crystal habit, characterization and pharmacological activity of various crystal forms of arteether

    Directory of Open Access Journals (Sweden)

    Renu Chadha

    2011-08-01

    Full Text Available The aim of this study was to investigate and characterize different crystal forms of arteether, a rapidly acting, highly potent antimalarial drug for the treatment of acute Plasmodium falciparum malaria. Six different crystal forms were prepared utilizing various polar and non-polar solvents. Scanning electron microscopy (SEM revealed differences in the surface characteristics of the six forms from those of a commercial sample. Differential scanning calorimetry (DSC revealed the absence of a desolvation endotherm indicating that the forms were neither hydrates nor solvates. Powder X-ray diffraction (PXRD patterns of the forms showed much weaker major peaks than in the commercial sample indicating them to be less crystalline. Solubility and dissolution studies showed that the most amorphous form was the most soluble and possessed the highest antimalarial activity.

  2. Theoretically informed Monte Carlo simulation of liquid crystals by sampling of alignment-tensor fields

    Energy Technology Data Exchange (ETDEWEB)

    Armas-Pérez, Julio C.; Londono-Hurtado, Alejandro [Institute for Molecular Engineering, University of Chicago, Chicago, Illinois 60637 (United States); Guzmán, Orlando [Departamento de Física, Universidad Autónoma Metropolitana, Iztapalapa, DF 09340, México (Mexico); Hernández-Ortiz, Juan P. [Departamento de Materiales y Minerales, Universidad Nacional de Colombia, Sede Medellín, Medellín (Colombia); Institute for Molecular Engineering, University of Chicago, Chicago, Illinois 60637 (United States); Pablo, Juan J. de, E-mail: depablo@uchicago.edu [Institute for Molecular Engineering, University of Chicago, Chicago, Illinois 60637 (United States); Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    2015-07-28

    A theoretically informed coarse-grained Monte Carlo method is proposed for studying liquid crystals. The free energy functional of the system is described in the framework of the Landau-de Gennes formalism. The alignment field and its gradients are approximated by finite differences, and the free energy is minimized through a stochastic sampling technique. The validity of the proposed method is established by comparing the results of the proposed approach to those of traditional free energy minimization techniques. Its usefulness is illustrated in the context of three systems, namely, a nematic liquid crystal confined in a slit channel, a nematic liquid crystal droplet, and a chiral liquid crystal in the bulk. It is found that for systems that exhibit multiple metastable morphologies, the proposed Monte Carlo method is generally able to identify lower free energy states that are often missed by traditional approaches. Importantly, the Monte Carlo method identifies such states from random initial configurations, thereby obviating the need for educated initial guesses that can be difficult to formulate.

  3. Theoretically informed Monte Carlo simulation of liquid crystals by sampling of alignment-tensor fields.

    Energy Technology Data Exchange (ETDEWEB)

    Armas-Perez, Julio C.; Londono-Hurtado, Alejandro; Guzman, Orlando; Hernandez-Ortiz, Juan P.; de Pablo, Juan J.

    2015-07-27

    A theoretically informed coarse-grained Monte Carlo method is proposed for studying liquid crystals. The free energy functional of the system is described in the framework of the Landau-de Gennes formalism. The alignment field and its gradients are approximated by finite differences, and the free energy is minimized through a stochastic sampling technique. The validity of the proposed method is established by comparing the results of the proposed approach to those of traditional free energy minimization techniques. Its usefulness is illustrated in the context of three systems, namely, a nematic liquid crystal confined in a slit channel, a nematic liquid crystal droplet, and a chiral liquid crystal in the bulk. It is found that for systems that exhibit multiple metastable morphologies, the proposed Monte Carlo method is generally able to identify lower free energy states that are often missed by traditional approaches. Importantly, the Monte Carlo method identifies such states from random initial configurations, thereby obviating the need for educated initial guesses that can be difficult to formulate.

  4. Correlation between Sweet Spots of Glycopeptides and Polymorphism of the Matrix Crystal in MALDI Samples.

    Science.gov (United States)

    Nishikaze, Takashi; Okumura, Hisako; Jinmei, Hiroshi; Amano, Junko

    2012-01-01

    A standard dried-droplet preparation using 2,5-dihydroxybenzoic acid (2,5-DHBA) as the matrix results in a large variation in signal intensity and poor shot-to-shot reproducibility in matrix-assisted laser desorption/ionization (MALDI). We expected that the differences can be attributed to the nature of the crystal structures in the region of the "sweet spot" within the MALDI samples. 2,5-DHBA crystals with and without analytes on a target plate obtained by means of a dried-droplet preparation contain two polymorphs, which can be distinguished by Raman spectra. In comparing the Raman image with the MS image, a clear correlation between the signal distribution of glycopeptides and hydrophilic peptides and the specific crystal form of 2,5-DHBA could be made. The ionization of hydrophobic peptides appears to proceed in both types of polymorphic crystals. In addition, the derivatization of glycopeptides with a pyrene group enabled us to detect glycopeptides regardless the crystal form. As the result, the number of sweet spots increased and MS spectra with a high signal intensity were obtained. The results suggest that the introduction of a hydrophobic/aromatic moiety to glycopeptides results in a more successful MALDI analysis due to the effective incorporation of the analyte into matrix crystals.

  5. Effect of method of crystallization on the IV-III and IV-II polymorphic transitions of ammonium nitrate.

    Science.gov (United States)

    Vargeese, Anuj A; Joshi, Satyawati S; Krishnamurthy, V N

    2009-01-15

    A study has been undertaken on the effect of crystallization method on the IVIII transition of ammonium nitrate (AN). AN is crystallized in three different ways, viz. recrystallization, evaporative crystallization and melt crystallization. When the samples were crystallized from saturated aqueous solution, ideal crystals were formed, which behaved differently from the crystals formed from the other methods. The DTA examination of the crystals showed that the crystals have different transition behaviour. The moisture uptake of the samples determined were found to have influenced by the mode of crystallization. The samples were further analyzed by powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). The present study showed that the parameters like thermal history, number of previous transformations and moisture content have a very negligible influence on the IVIII transition of AN as compared to the method of crystallization.

  6. Chiral crystal of a C2v-symmetric 1,3-diazaaulene derivative showing efficient optical second harmonic generation

    KAUST Repository

    Ma, Xiaohua

    2011-03-01

    Achiral nonlinear optical (NLO) chromophores 1,3-diazaazulene derivatives, 2-(4â€-aminophenyl)-6-nitro-1,3-diazaazulene (APNA) and 2-(4â€-N,N-diphenylaminophenyl)-6-nitro-1,3-diazaazulene (DPAPNA), were synthesized with high yield. Despite the moderate static first hyperpolarizabilities (β0) for both APNA [(136 ± 5) à - 10-30 esu] and DPAPNA [(263 ± 20) à - 10-30 esu], only APNA crystal shows a powder efficiency of second harmonic generation (SHG) of 23 times that of urea. It is shown that the APNA crystallization driven cooperatively by the strong H-bonding network and the dipolar electrostatic interactions falls into the noncentrosymmetric P2 12121 space group, and that the helical supramolecular assembly is solely responsible for the efficient SHG response. To the contrary, the DPAPNA crystal with centrosymmetric P-1 space group is packed with antiparalleling dimmers, and is therefore completely SHG-inactive. 1,3-Diazaazulene derivatives are suggested to be potent building blocks for SHG-active chiral crystals, which are advantageous in high thermal stability, excellent near-infrared transparency and high degree of designing flexibility. © 2011 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys, 2011 Optical crystals based on 1,3-diazaazulene derivatives are reported as the first example of organic nonlinear optical crystal whose second harmonic generation activity is found to originate solely from the chirality of their helical supramolecular orientation. The strong H-bond network forming between adjacent choromophores is found to act cooperatively with dipolar electrostatic interactions in driving the chiral crystallization of this material. Copyright © 2011 Wiley Periodicals, Inc.

  7. Durability of building stones against artificial salt crystallization

    Science.gov (United States)

    Min, K.; Park, J.; Han, D.

    2005-12-01

    Salts have been known as the most powerful weathering agents, especially when combined with frost action. Salt crystallization test along with freezing-thawing test and acid immersion test was carried out to assess the durability of building stones against weathering. Granite, limestone, marble and basalt were sampled from different quarries in south Korea for this study. One cycle of artificial salt crystallization test was composed of immersion of cored rock specimens in oversaturated solutions of CaCl2, KCl, NaCl and Na2SO4, respectively for 15 hours and successive drying in an oven of 105°C for 3 hours and cooling at room temperature. Tests were performed up to 30 cycles, and specific gravity and ultrasonic velocity were measured after experiencing every 10 cycles and uniaxial compressive strength was measured only after 30 cycles. During the repeated Na2SO4 salt crystallization, some rock samples were gradually deformed excessively and burst after 20 to 30 cycles of test. The variation patterns of physical properties during the salt crystallization tests are too variable to generalize the effect of salt weathering on physical properties but limestone, marble and basalt samples showed relatively greater change of physical properties than granite samples. The recrystallized salts were well observed in the cracks of rock samples through the scanning electron microscope. In the all salt crystallization tests, apparent specific gravities for all tested samples increased generally but not so significantly due to recrystallization of salts. It can be inferred that filling the pores with salt crystals cause the increase of ultrasonic velocity during the early stage of salt crystallization and then in later stages the repeated cycles of salt crystallization result in development of cracks leading decrease of ultrasonic velocity for some rock samples.

  8. Spherical Nb single crystals containerlessly grown by electrostatic levitation

    International Nuclear Information System (INIS)

    Sung, Y.S.; Takeya, H.; Hirata, K.; Togano, K.

    2003-01-01

    Spherical Nb (T m =2750 K) single crystals were grown via containerless electrostatic levitation (ESL). Samples became spherical at melting in levitation and undercooled typically 300-450 K prior to nucleation. As-processed samples were still spherical without any macroscopic shape change by solidification showing a uniform dendritic surface morphology. Crystallographic {111} planes exposed in equilateral triangular shapes on the surface by preferential macroetching and spotty back-reflection Laue patterns confirm the single crystal nature of the ESL-processed Nb samples. No hysteresis in magnetization between zero field and field cooling also implies a clean defect-free condition of the spherical Nb single crystals

  9. Ice crystal precipitation at Dome C site (East Antarctica)

    Science.gov (United States)

    Santachiara, G.; Belosi, F.; Prodi, F.

    2016-01-01

    For the first time, falling ice crystals were collected on glass slides covered with a thin layer of 2% formvar in chloroform at the Dome Concordia site (Dome C), Antarctica. Samplings were performed in the framework of the 27th Italian Antarctica expedition of the Italian National Program for Research in Antarctica in the period 21 February-6 August 2012. Events of clear-sky precipitations and precipitations from clouds were considered and the replicas obtained were examined under Scanning Electron Microscope (SEM). Several shapes of ice crystals were identified, including ;diamond dust; (plates, pyramids, hollow and solid columns), and crystal aggregates varying in complexity. Single events often contained both small (10 μm to 50 μm) and large (hundreds of microns) crystals, suggesting that crystals can form simultaneously near the ground (height of a few hundred metres) and at higher layers (height of thousands of metres). Images of sampled crystal replicas showed that single bullets are not produced separately, but by the disintegration of combinations of bullets. Rimed ice crystals were absent in the Dome C samples, i.e. the only mode of crystal growth was water vapour diffusion. On considering the aerosol in the sampled crystals, we reached the conclusion that inertial impaction, interception and Brownian motion were insufficient to explain the scavenged aerosol. We therefore presume that phoretic forces play a role in scavenging during the crystal growth process.

  10. Monomial Crystals and Partition Crystals

    Science.gov (United States)

    Tingley, Peter

    2010-04-01

    Recently Fayers introduced a large family of combinatorial realizations of the fundamental crystal B(Λ0) for ^sln, where the vertices are indexed by certain partitions. He showed that special cases of this construction agree with the Misra-Miwa realization and with Berg's ladder crystal. Here we show that another special case is naturally isomorphic to a realization using Nakajima's monomial crystal.

  11. Irradiation damage of alkali halide crystals during positron bombardment

    International Nuclear Information System (INIS)

    Arefiev, K.P.; Arefiev, V.P.; Vorobiev, S.A.

    1978-01-01

    The bleaching effect of positron irradiation of KCl and KBr single crystals previously coloured with electrons or protons was investigated. Positrons injection in the coloured alkali halide samples reduced the F-centres concentration considerably. For KCl crystals thicker than the positrons range the appearance of additional bands in the absorption spectra is noticeable. The experimental data show that the bleaching phenomenon should be observed merely throughout the positron exposure both for irradiated and non-irradiated regions of the sample. Irradiation effects, due to positron source, on the peak counting rate of (γ-γ) angular correlation in KCl crystals under applied magnetic field were also investigated. The growth of peak counting rate shows the increase of positronium-like states formation near defects of cation sublattice. (author)

  12. CRYSTALLIZATION KINETICS OF GLASS-CERAMICS BY DIFFERENTIAL THERMAL ANALYSIS

    Directory of Open Access Journals (Sweden)

    A. NOZAD

    2011-06-01

    Full Text Available The crystallization behavior of fluorphlogopite, a glass-ceramic in the MgO–SiO2–Al2O3–K2O–B2O3–F system, was studied by substitution of Li2O for K2O in the glass composition. DTA, XRD and SEM were used for the study of crystallization behavior, formed phases and microstructure of the resulting glass-ceramics. Crystallization kinetics of the glass was investigated under non-isothermal conditions, using the formal theory of transformations for heterogeneous nucleation. The crystallization results were analyzed, and both the activation energy of crystallization process as well as the crystallization mechanism were characterized. Calculated kinetic parameters indicated that the appropriate crystallization mechanism was bulk crystallization for base glass and the sample with addition of Li2O. Non-isothermal DTA experiments showed that the crystallization activation energies of base glasses was in the range of 234-246 KJ/mol and in the samples with addition of Li2O was changed to the range of 317-322 KJ/mol.

  13. Nematic liquid crystal in a cylindrical sample: Theoretical analysis of the electrical response

    Science.gov (United States)

    Gomes, O. A.; Yednak, C. A. R.; da Silva, B. V. H. V.; Teixeira-Souza, R. T.

    2018-02-01

    The electrical responses of a nematic liquid crystal sample confined between two cylindrical surfaces are investigated in the framework of elastic continuum theory. The responses are the result of the molecular reorientation induced by both the applied electric field and the cylindrical geometry of the sample. The nematic medium is considered as a parallel RC circuit since the capacitance and the resistance are under the same difference of potential. The electrical properties, including the total electric current, are determined from the molecular reorientation of the director. The elastic anisotropy has been shown to influence substantially the profile of the electrical current, capacitance, and resistance characterizing the equivalent circuit for the medium.

  14. Fano resonance in anodic aluminum oxide based photonic crystals.

    Science.gov (United States)

    Shang, Guo Liang; Fei, Guang Tao; Zhang, Yao; Yan, Peng; Xu, Shao Hui; Ouyang, Hao Miao; Zhang, Li De

    2014-01-08

    Anodic aluminum oxide based photonic crystals with periodic porous structure have been prepared using voltage compensation method. The as-prepared sample showed an ultra-narrow photonic bandgap. Asymmetric line-shape profiles of the photonic bandgaps have been observed, which is attributed to Fano resonance between the photonic bandgap state of photonic crystal and continuum scattering state of porous structure. And the exhibited Fano resonance shows more clearly when the sample is saturated ethanol gas than air-filled. Further theoretical analysis by transfer matrix method verified these results. These findings provide a better understanding on the nature of photonic bandgaps of photonic crystals made up of porous materials, in which the porous structures not only exist as layers of effective-refractive-index material providing Bragg scattering, but also provide a continuum light scattering state to interact with Bragg scattering state to show an asymmetric line-shape profile.

  15. Synthesis of electro-optically active polymer composite of poly[2,2'-bis(3,4-ethylenedioxythiophene-alt-fluorene]/hydroxypropyl cellulose showing liquid crystal structure

    Directory of Open Access Journals (Sweden)

    N. Eguchi

    2017-10-01

    Full Text Available Electrochemical preparation of a composite consisting of poly[2,2′-bis(3,4-ethylenedioxythiophene-alt-fluorene] and hydroxypropyl cellulose (PEFE/HPC was carried out. We conducted electrochemical polymerization of poly[2,2′-bis(3,4-ethylenedioxythiophene-alt-fluorene] (EFE as a monomer in a lyotropic liquid crystal of HPC. We used an organic solvent instead of water for lyotropic liquid crystal medium to expand the possibility of the range of monomers, although water is usually employed as a solvent for HPC for showing liquid crystallinity. Here, we employed N,N-dimethylformamide (DMF as a solvent for HPC. Electrochemical polymerization in the polymer liquid crystal was carried out to obtain a polymer film with liquid crystal order. The polymer film thus prepared exhibited optical activity. Fourier transfer infrared (FT-IR absorption spectroscopy reveals that the film is a composite consisting of HPC and polymer. The composite PEFE/HPC thus prepared in HPC/DMF system showed electrochromism.

  16. An FPGA-based Sampling-ADC readout for the crystal barrel calorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Muellers, Johannes [Helmholtz-Institut fuer Strahlen- und Kernphysik, Bonn (Germany); Marciniewski, Pawel [Angstroemlaboratoriet, Uppsala (Sweden); Collaboration: CBELSA/TAPS-Collaboration

    2016-07-01

    The CBELSA/TAPS experiment at the electron accelerator ELSA (Bonn) investigates the photoproduction of mesons off protons and neutrons. The Crystal Barrel Calorimeter has been upgraded replacing its photodiode readout by APDs, which allows the integration of the calorimeter into the first level trigger. Since the possible DAQ rate is currently limited by the digitization stage (LeCroy QDC1885F) to ∼ 2 kHz, the implementation of a new Sampling-ADC (SADC) readout is the second important step in the upgrade of the detector system. Based on the 64-channel PANDA-SADC, the design was modified, adapting it to the needs of the CBELSA/TAPS experiment. The CB-SADC offers 64 channels in one NIM module with up to 14 bit rate at 125 MHz, accompanied by a modular analog input stage and power supply. Data processing and reduction are realized with Kintex7 FPGAs. Readout is possible via gigabit ethernet links. Using an FPGA provides a multitude of possibilities for online feature extraction, such as the determination of the energy deposited in the crystal, TDC capabilities and pile-up detection and recovery. The SADC development is discussed, and first measurements performed in comparison to the presently used LeCroy QDC are presented.

  17. Spinel-rich lithologies in the lunar highland crust: Linking lunar samples, crystallization experiments and remote sensing

    Science.gov (United States)

    Gross, J.; Treiman, A. H.

    2012-12-01

    The discovery of areas rich in (Mg,Fe)-Al spinel on the rims and central peaks of lunar impact basins (by the M3 mapping spectrometer on Chandrayaan-1) has revived the old puzzle of the origin of lunar spinel. (Mg,Fe)-Al spinel is rare but widespread in lunar highlands rocks, and thus might be an important component of the lunar crust [1-3]. However, the origin of this spinel is not clear. Lunar (Mg,Fe)-Al spinel could have formed (1) during 'normal' basalt petrogenesis at high pressure; (2) during low-pressure crystallization of melts rich in olivine and plagioclase components, e.g. impact-melted lunar troctolite; or (3) formed at low pressure during assimilation of anorthosite into picritic magma; thus, lunar spinel-rich areas represent old (pre-impact) intrusions of magma. In the absence of spinel-rich samples from the Moon, however, these ideas have been highly speculative. Here we describe a rock fragment from lunar meteorite ALHA 81005 that we recently reported [4] that not only contains spinel, but is the first spinel-rich lunar sample described. This fragment contains ~30% (Mg,Fe)Al spinel and is so fine grained that it reasonably could represent a larger rock body. However, the fragment is so rich in spinel that it could not have formed by melting a peridotitic mantle or a basaltic lunar crust. The clast's small grain size and its apparent disequilibrium between spinel and pyroxene suggest fairly rapid crystallization at low pressure. It could have formed as a spinel cumulate from an impact melt of troctolitic composition; or from a picritic magma that assimilated crustal anorthosite on its margins. The latter mechanism is preferred because it explains the petrographic and chemical features of our clast, and is consistent with the regional setting of the Moscoviense spinel deposit [4]. To better understand the origin and formation history(s) of spinel-rich rocks, we also performed liquidus/crystallization experiments at low-pressure as analogues for impact

  18. Chiral crystal of a C2v-symmetric 1,3-diazaaulene derivative showing efficient optical second harmonic generation

    KAUST Repository

    Ma, Xiaohua; Fu, Limin; Zhao, Yunfeng; Ai, Xicheng; Zhang, Jianping; Han, Yu; Guo, Zhixin

    2011-01-01

    the moderate static first hyperpolarizabilities (β0) for both APNA [(136 ± 5) à - 10-30 esu] and DPAPNA [(263 ± 20) à - 10-30 esu], only APNA crystal shows a powder efficiency of second harmonic generation (SHG) of 23 times that of urea. It is shown

  19. Preventing Crystal Agglomeration of Pharmaceutical Crystals Using Temperature Cycling and a Novel Membrane Crystallization Procedure for Seed Crystal Generation

    Directory of Open Access Journals (Sweden)

    Elena Simone

    2018-01-01

    Full Text Available In this work, a novel membrane crystallization system was used to crystallize micro-sized seeds of piroxicam monohydrate by reverse antisolvent addition. Membrane crystallization seeds were compared with seeds produced by conventional antisolvent addition and polymorphic transformation of a fine powdered sample of piroxicam form I in water. The membrane crystallization process allowed for a consistent production of pure monohydrate crystals with narrow size distribution and without significant agglomeration. The seeds were grown in 350 g of 20:80 w/w acetone-water mixture. Different seeding loads were tested and temperature cycling was applied in order to avoid agglomeration of the growing crystals during the process. Focused beam reflectance measurement (FBRM; and particle vision and measurement (PVM were used to monitor crystal growth; nucleation and agglomeration during the seeded experiments. Furthermore; Raman spectroscopy was used to monitor solute concentration and estimate the overall yield of the process. Membrane crystallization was proved to be the most convenient and consistent method to produce seeds of highly agglomerating compounds; which can be grown via cooling crystallization and temperature cycling.

  20. Design and Development of a Robot-Based Automation System for Cryogenic Crystal Sample Mounting at the Advanced Photon Source

    International Nuclear Information System (INIS)

    Shu, D.; Preissner, C.; Nocher, D.; Han, Y.; Barraza, J.; Lee, P.; Lee, W.-K.; Cai, Z.; Ginell, S.; Alkire, R.; Lazarski, K.; Schuessler, R.; Joachimiak, A.

    2004-01-01

    X-ray crystallography is the primary method to determine the 3D structures of complex macromolecules at high resolution. In the years to come, the Advanced Photon Source (APS) and similar 3rd-generation synchrotron sources elsewhere will become the most powerful tools for studying atomic structures of biological molecules. One of the major bottlenecks in the x-ray data collection process is the constant need to change and realign the crystal sample. This is a very time- and manpower-consuming task. An automated sample mounting system will help to solve this bottleneck problem. We have developed a novel robot-based automation system for cryogenic crystal sample mounting at the APS. Design of the robot-based automation system, as well as its on-line test results at the Argonne Structural Biology Center (SBC) 19-BM experimental station, are presented in this paper

  1. Crystal growth of YFe{sub 2}Ge{sub 2} and the dependence of its superconducting properties on sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Jiasheng; Semeniuk, Konstantin; Reiss, Pascal; Brown, Philip; Grosche, Malte [Cavendish Lab., Cambridge (United Kingdom); Feng, Zhuo [London Centre of Nanotechnology, UCL, London (United Kingdom); Lampronti, Giulio [Cambridge Univ., Dept. of Earth Sciences, Cambridge (United Kingdom)

    2016-07-01

    The d-electron system YFe{sub 2}Ge{sub 2} exhibits an unusually high Sommerfeld ratio of specific heat capacity of C/T ∝ 100 mJ/(molK{sup 2}), signaling strong electronic correlations. Evidence of superconductivity has been reported in polycrystals and in flux-grown single crystals with residual resistance ratios (RRR) of the order of 50, but these samples show no thermodynamic signatures of a bulk superconducting transition. We find that by combining (i) a prereaction of YFe{sub 2}, (ii) careful control of nominal composition, and (iii) subsequent annealing procedures, the polycrystalline YFe{sub 2}Ge{sub 2} samples grown using a radio-frequency (RF) induction furnace can reach RRR values ∝ 200 with resistive superconducting transitions temperatures of around 1.85 K. This new generation of sample displays clear heat capacity anomalies as well as nearly 100% diamagnetic screening, confirming the bulk nature of its superconductivity. We present details of the sample preparation and characterization and discuss the correlation between nominal composition and superconductivity.

  2. Ball-milling-induced crystallization and ball-milling effect on thermal crystallization kinetics in an amorphous FeMoSiB alloy

    International Nuclear Information System (INIS)

    Guo, F.Q.; Lu, K.

    1997-01-01

    Microstructure evolution in a melt-spun amorphous Fe 77.2 Mo 0.8 Si 9 B 13 alloy subjected to high-energy ball milling was investigated by means of X-ray diffraction (XRD), a transmission electron microscope (TEM), and a differential scanning calorimeter (DSC). It was found that during ball milling, crystallization occurs in the amorphous ribbon sample with precipitation of an α-Fe solid solution, and the amorphous sample crystallizes completely into a single α-Fe nanostructure (rather than α-Fe and borides as in the usual thermal crystallization products) when the milling time exceeds 135 hours. The volume fraction of material crystallized was found to be approximately proportional to the milling time. The fully crystallized sample with a single α-Fe nanophase exhibits an intrinsic thermal stability against phase separation upon annealing at high temperatures. The ball-milling effect on the subsequent thermal crystallization of the amorphous phase in an as-milled sample was studied by comparison of the crystallization products and kinetic parameters between the as-quenched amorphous sample and the as-milled sample was studied by comparison of the crystallization products and kinetic parameters between the as-quenched amorphous sample and the as-milled partially crystallized samples. The crystallization temperatures and activation energies for the crystallization processes of the residual amorphous phase were considerably decreased due to ball milling, indicating that ball milling has a significant effect on the depression of thermal stability of the residual amorphous phase

  3. Electrical conductivity of high-purity germanium crystals at low temperature

    Science.gov (United States)

    Yang, Gang; Kooi, Kyler; Wang, Guojian; Mei, Hao; Li, Yangyang; Mei, Dongming

    2018-05-01

    The temperature dependence of electrical conductivity of single-crystal and polycrystalline high-purity germanium (HPGe) samples has been investigated in the temperature range from 7 to 100 K. The conductivity versus inverse of temperature curves for three single-crystal samples consist of two distinct temperature ranges: a high-temperature range where the conductivity increases to a maximum with decreasing temperature, and a low-temperature range where the conductivity continues decreasing slowly with decreasing temperature. In contrast, the conductivity versus inverse of temperature curves for three polycrystalline samples, in addition to a high- and a low-temperature range where a similar conductive behavior is shown, have a medium-temperature range where the conductivity decreases dramatically with decreasing temperature. The turning point temperature ({Tm}) which corresponds to the maximum values of the conductivity on the conductivity versus inverse of temperature curves are higher for the polycrystalline samples than for the single-crystal samples. Additionally, the net carrier concentrations of all samples have been calculated based on measured conductivity in the whole measurement temperature range. The calculated results show that the ionized carrier concentration increases with increasing temperature due to thermal excitation, but it reaches saturation around 40 K for the single-crystal samples and 70 K for the polycrystalline samples. All these differences between the single-crystal samples and the polycrystalline samples could be attributed to trapping and scattering effects of the grain boundaries on the charge carriers. The relevant physical models have been proposed to explain these differences in the conductive behaviors between two kinds of samples.

  4. Femtosecond X-ray diffraction from two-dimensional protein crystals

    Directory of Open Access Journals (Sweden)

    Matthias Frank

    2014-03-01

    Full Text Available X-ray diffraction patterns from two-dimensional (2-D protein crystals obtained using femtosecond X-ray pulses from an X-ray free-electron laser (XFEL are presented. To date, it has not been possible to acquire transmission X-ray diffraction patterns from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permit a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy approach at the Linac Coherent Light Source, Bragg diffraction was acquired to better than 8.5 Å resolution for two different 2-D protein crystal samples each less than 10 nm thick and maintained at room temperature. These proof-of-principle results show promise for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.

  5. Design of Agglomerated Crystals of Ibuprofen During Crystallization: Influence of Surfactant

    Directory of Open Access Journals (Sweden)

    Maryam Maghsoodi

    2011-01-01

    Full Text Available Objective(sIbuprofen is a problematic drug in tableting, and dissolution due to its poor solubility, hydrophobicity, and tendency to stick to surface. Because of the bad compaction behavior ibuprofen has to be granulated usually before tableting. However, it would be more satisfactory to obtain directly during the crystallization step crystalline particles that can be directly compressed and quickly dissolved. Materials and Methods Crystallization of ibuprofen was carried out using the quasi emulsion solvent diffusion method in presence of surfactant (sodium lauryl sulfate (SLS, Tween 80. The particles were characterized by differential scanning calorimetry (DSC, powder X-ray diffraction (XRPD and were evaluated for particle size, flowability, drug release and tableting behavior. ResultsIbuprofen particles obtained in the presence of surfactants consisted of numerous plate- shaped crystals which had agglomerated together as near spherical shape. The obtained agglomerates exhibited significantly improved micromeritic properties as well as tableting behavior than untreated drug crystals. The agglomerates size and size distribution was largely controlled by surfactant concentration, but there was no significant influence found on the tableting properties. The dissolution tests showed that the agglomerates obtained in presence of SLS exhibited enhanced dissolution rate while the agglomerates made in the presence of Tween 80 had no significant impact on dissolution rate of ibuprofen in comparison to untreated sample. The XRPD and DSC results showed that during the agglomeration process, ibuprofen did not undergo any polymorphic changes.Conclusion The study highlights the influence of surfactants on crystallization process leading to modified performance.

  6. The facile and low temperature synthesis of nanophase hydroxyapatite crystals using wet chemistry

    International Nuclear Information System (INIS)

    Dhand, Vivek; Rhee, K.Y.; Park, Soo-Jin

    2014-01-01

    A simple and facile wet chemistry route was used to synthesize nanophase hydroxyapatite (HaP) crystals at low temperature. The synthesis was carried out at a pH of 11.0 and at a temperature of 37 °C. The resulting samples were washed several times and subjected to further analysis. XRD studies revealed that the HaP crystals were polycrystalline in nature with a crystallite size of ∼ 15–60 ± 5 nm. SEM-EDXA images confirmed the presence of calcium (Ca), phosphorous (P), and oxygen (O) peaks. Likewise, FTIR confirmed the presence of characteristic phosphate and hydroxyl peaks in samples. Lastly, HRTEM images clearly showed distinctive lattice fringes positioned in the 100 and 002 planes. TGA analysis shows that HaP crystals can withstand higher calcination temperatures and are thermally stable. - Highlights: • Facile and low temperature nanophase HaP crystals synthesized at pH 11 and 37 °C • Electron microscopy image of HaP shows characteristic rice grain like morphology. • FTIR results show the characteristic and fingerprint functional groups of HaP. • Thermal stability of HaP crystals up to 500 °C • Growth of Hap crystals occur parallel to c-axis and a possible mechanism proposed

  7. Characterizing full matrix constants of piezoelectric single crystals with strong anisotropy using two samples

    Science.gov (United States)

    Tang, Liguo; Zhang, Yang; Cao, Wenwu

    2016-10-01

    Although the self-consistency of the full matrix material constants of a piezoelectric sample obtained by the resonant ultrasonic spectroscopy technique can be guaranteed because all constants come from the same sample, it is a great challenge to determine the constants of a piezoelectric sample with strong anisotropy because it might not be possible to identify enough resonance modes from the resonance spectrum. To overcome this difficulty, we developed a strategy to use two samples of similar geometries to increase the number of easy identifiable modes. Unlike the IEEE resonance methods, sample-to-sample variation here is negligible because the two samples have almost the same dimensions, cut from the same specimen and poled under the same conditions. Using this method, we have measured the full matrix constants of a [011]c poled 0.71Pb(Mg1/3Nb2/3)O3-0.29PbTiO3 single crystal, which has 17 independent constants. The self-consistency of the obtained results is checked by comparing the calculated elastic stiffness constants c33 D , c44 D , and c55 D with those directly measured ones using the ultrasonic pulse-echo method.

  8. Effect of indium and antimony doping in SnS single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Chaki, Sunil H., E-mail: sunilchaki@yahoo.co.in; Chaudhary, Mahesh D.; Deshpande, M.P.

    2015-03-15

    Highlights: • Single crystals growth of pure SnS, indium doped SnS and antimony doped SnS by direct vapour transport (DVT) technique. • Doping of In and Sb occurred in SnS single crystals by cation replacement. • The replacement mechanism ascertained by EDAX, XRD and substantiated by Raman spectra analysis. • Dopants concentration affects the optical energy bandgap. • Doping influences electrical transport properties. - Abstract: Single crystals of pure SnS, indium (In) doped SnS and antimony (Sb) doped SnS were grown by direct vapour transport (DVT) technique. Two doping concentrations of 5% and 15% each were employed for both In and Sb dopants. Thus in total five samples were studied viz., pure SnS (S1), 5% In doped SnS (S2), 15% In doped SnS (S3), 5% Sb doped SnS (S4) and 15% Sb doped SnS (S5). The grown single crystal samples were characterized by evaluating their surface microstructure, stoichiometric composition, crystal structure, Raman spectroscopy, optical and electrical transport properties using appropriate techniques. The d.c. electrical resistivity and thermoelectric power variations with temperature showed semiconducting and p-type nature of the as-grown single crystal samples. The room temperature Hall Effect measurements further substantiated the semiconducting and p-type nature of the as-grown single crystal samples. The obtained results are deliberated in detail.

  9. Isothermal Crystallization Kinetics of HDPE/HA Compounds Irradiated with Sterilization Doses of Gamma Rays

    International Nuclear Information System (INIS)

    Albano, C.

    2006-01-01

    The objective of this work was to study the isothermal crystallization of High Density Polyethylene/Hydroxyapatite nanocomposites, with 2 and 5 ppc of HA, irradiated with 25 kGy (sterilization dose) of γ-Ray from a 60 C o source, at a rate of 4.8 kGy/h in air and at room temperature. The selected crystallization temperatures were 118, 117, 116 and 115 degree. The crystallization kinetics was analyzed using the Avrami's model whose parameters were optimized using a non-linear regression technique. Regression results show that the Avrami exponent varies between 1.8 and 1.5, meaning that the spherulitic growth is mainly two dimensional. Values for specific crystallization constant 'k' were found to be higher for HDPE/HA compounds than for pure HDPE, clearly indicating the presence of an HA nucleation effect. It was also observed that values for the specific crystallization constant 'k' decreases with increasing temperatures, being this effect more noticeable for HDPE/HA compounds than for pure HDPE. Regarding to irradiated samples, their 'k' values were found to be lower than those for non irradiated samples, the difference getting more significant with decreasing crystallization temperature. Simulation of experimental data with the Avrami's model show a clear influence of the crystallization temperature, the HA content in the sample and the amount of applied radiation. It was also observed that the Avrami model correlates satisfactorily experimental data for not irradiated samples of pure HDPE and HDPE/HA compounds at the highest crystallization (T c ). However, as the crystallization temperature decreases, the values simulated with the Avrami model increasingly deviate from experimental data, specifically at the highest values of the relative crystallinity. This effect is even stronger on irradiated samples of HDPE and HDPE/HA compounds

  10. Structural coloration of chitosan-cationized cotton fabric using photonic crystals

    Science.gov (United States)

    Yavuz, G.; Zille, A.; Seventekin, N.; Souto, A. P.

    2017-10-01

    In this work, poly (styrene-methyl methacrylate-acrylic acid) P(St-MMA-AA) composite nanospheres were deposited onto chitosan-cationized woven cotton fabrics followed by a second layer of chitosan. The deposited photonic crystals (PCs) on the fabrics were evaluated for coating efficiency and resistance, chemical analysis and color variation by optical and SEM microscopy, ATR-FTIR, diffuse reflectance spectroscopy and washing fastness. Chitosan deposition on cotton fabric provided cationic groups on the fiber surface promoting electrostatic interaction with photonic crystals. SEM images of the washed samples indicate that the PCs are firmly coated on the cotton surface only in the chitosan treated sample. The photonic nanospheres show an average diameter of 280 nm and display a face-centered cubic closepacking structure with an average thickness of 10 μm. A further chitosan post-treatment enhances color yield of the samples due to the chitosan transparent covering layer that induce bright reflections where the angles of incidence and reflection are the same. After washing, no photonic crystal can be detected on control fabric surface. However, the sample that received a chitosan post-treatment showed a good washing fastness maintaining a reasonable degree of iridescence. Chitosan fills the spaces between the polymer spheres in the matrix stabilizing the photonic structure. Sizeable variations in lattice spacing will allow color variations using more flexible non-close-packed photonic crystal arrays in chitosan hydrogels matrices.

  11. Single-crystal growth of ceria-based materials

    International Nuclear Information System (INIS)

    Ulbrich, Gregor

    2015-01-01

    In this work it could be shown that Skull-Melting is a suitable method for growing ceria single crystals. Twenty different ceria-based single crystals could be manufactured. It was possible to dope ceria single crystals with Gd, Sm, Y, Zr, Ti, Ta, and Pr in different concentrations. Also co-doping with the named metals was realized. However, there remain some problems for growing ceria-based single crystals by Skull-Melting. As ignition metal zirconium was used because no ceria-based material works well. For that reason all single crystals show small zirconium contamination. Another problem is the formation of oxygen by the heat-induced reduction of ceria during the melting process. Because of that the skull of sintered material is often destroyed by gas pressure. This problem had to be solved individually for every single crystal. The obtained single crystals were characterized using different methods. To ensure the single crystal character the y were examined by Laue diffraction. All manufactured crystals are single crystals. Also powder diffraction patterns of the milled and oxidized samples were measured. For the determination of symmetry and metric the structural parameters were analyzed by the Rietveld method. All synthesized materials crystallize in space group Fm-3m known from calcium fluoride. The cubic lattice parameter a was determined for all crystals. In the case of series with different cerium and zirconium concentrations a linear correlation between cerium content and cubic lattice parameter was detected. The elemental composition was determined by WDX. All crystals show a homogeneous elemental distribution. The oxygen content was calculated because the WDX method isn't useful for determination.

  12. Rapid Crystallization of the Bishop Magma

    Science.gov (United States)

    Gualda, G. A.; Anderson, A. T.; Sutton, S. R.

    2007-12-01

    Substantial effort has been made to understand the longevity of rhyolitic magmas, and particular attention has been paid to the systems in the Long Valley area (California). Recent geochronological data suggest discrete magma bodies that existed for hundreds of thousands of years. Zircon crystallization ages for the Bishop Tuff span 100-200 ka, and were interpreted to reflect slow crystallization of a liquid-rich magma. Here we use the diffusional relaxation of Ti zoning in quartz to investigate the longevity of the Bishop magma. We have used such an approach to show the short timescales of crystallization of Ti-rich rims on quartz from early- erupted Bishop Tuff. We have now recognized Ti-rich cores in quartz that can be used to derive the timescales of their crystallization. We studied four samples of the early-erupted Bishop. Hand-picked crystals were mounted on glass slides and polished. Cathodoluminescence (CL) images were obtained using the electron microprobe at the University of Chicago. Ti zoning was documented using the GeoSoilEnviroCARS x-ray microprobe at the Advanced Photon Source (Argonne National Lab). Quartz crystals in all 4 samples include up to 3 Ti-bearing zones: a central core (50-100 μm in diameter, ca. 50 ppm Ti), a volumetrically predominant interior (~40 ppm Ti), and in some crystals a 50-100 μm thick rim (50 ppm Ti). Maximum estimates of core residence times were calculated using a 1D diffusion model, as the time needed to smooth an infinitely steep profile to fit the observed profile. Surprisingly, even for the largest crystals studied - ca. 2 mm in diameter - core residence times are less than 1 ka. Calculated growth rates imply that even cm-sized crystals crystallized in less than 10 ka. Crystal size distribution data show that crystals larger than 3 mm are exceedingly rare, such that the important inference is that the bulk of the crystallization of the early-erupted Bishop magma occurred in only a few thousand years. This timescale

  13. Influence of crystal habit on the compression and densification mechanism of ibuprofen

    Science.gov (United States)

    Di Martino, Piera; Beccerica, Moira; Joiris, Etienne; Palmieri, Giovanni F.; Gayot, Anne; Martelli, Sante

    2002-08-01

    Ibuprofen was recrystallized from several solvents by two different methods: addition of a non-solvent to a drug solution and cooling of a drug solution. Four samples, characterized by different crystal habit, were selected: sample A, sample E and sample T, recrystallized respectively from acetone, ethanol and THF by addition of water as non-solvent and sample M recrystallized from methanol by temperature decrease. By SEM analysis, sample were characterized with the respect of their crystal habit, mean particle diameter and elongation ratio. Sample A appears stick-shaped, sample E acicular with lamellar characteristics, samples T and M polyhedral. DSC and X-ray diffraction studies permit to exclude a polymorphic modification of ibuprofen during crystallization. For all samples micromeritics properties, densification behaviour and compression ability was analysed. Sample M shows a higher densification tendency, evidenciated by its higher apparent and tapped particle density. The ability to densificate is also pointed out by D0' value of Heckel's plot, which indicate the rearrangement of original particles at the initial stage of compression. This fact is related to the crystal habit of sample M, which is characterized by strongly smoothed coins. The increase in powder bed porosity permits a particle-particle interaction of greater extent during the subsequent stage of compression, which allows higher tabletability and compressibility.

  14. Adsorption of CO on, and S poisoning of, a perfect Ni(111) single crystal and a Ni(111) crystal with small angle boundaries

    Energy Technology Data Exchange (ETDEWEB)

    Sargent, G A; Freeman, G B; Chao, J L.R.

    1980-01-01

    A Ni(111) crystal with small angle boundaries was used to examine the adsorption of CO. The adsorption of CO on a perfect Ni(111) single crystal was used for reference. Auger spectra show that the boundary lines on the sample surface provide favorable sites for the adsorbed CO to dissociate at temperatures as low as 25/sup 0/C. The post-dissociation carbon appears mostly in the form of a nickel carbide on the surface. After heating the crystal to 850/sup 0/C, sulfur diffused to the surface and blocked the surface adsorption sites uniformly. The boundary-enhanced dissociation of absorbed CO is no longer observed after the diffusion of sulfur to the crystal surface. AES depth profiling of sulfur concentration at different positions on the crystal with respect to the boundary lines show no evidence that the boundary lines provide an enhanced path for sulfur diffusion. 7 figures.

  15. Ultrasonography shows disappearance of monosodium urate crystal deposition on hyaline cartilage after sustained normouricemia is achieved.

    Science.gov (United States)

    Thiele, Ralf G; Schlesinger, Naomi

    2010-02-01

    This study aimed at determining whether lowering serum urate (SU) to less than 6 mg/dl in patients with gout affects ultrasonographic findings. Seven joints in five patients with monosodium urate (MSU) crystal proven gout and hyperuricemia were examined over time with serial ultrasonography. Four of the five patients were treated with urate lowering drugs (ULDs) (allopurinol, n = 3; probenecid, n = 1). One patient was treated with colchicine alone. Attention was given to changes in a hyperechoic, irregular coating of the hyaline cartilage in the examined joints (double contour sign or "urate icing"). This coating was considered to represent precipitate of MSU crystals. Index joints included metacarpophalangeal (MCP) joints (n = 2), knee joints (n = 3), and first metatarsophalangeal (MTP) joints (n = 2). The interval between baseline and follow-up images ranged from 7 to 18 months. Serial SU levels were obtained during the follow-up period. During the follow-up period, three patients treated with ULD (allopurinol, n = 2; probenecid, n = 1) achieved a SU level of or =7 mg/dl. In one patient treated with allopurinol, SU levels improved from 13 to 7 mg/dl during the follow-up period. Decrease, but not resolution of the hyperechoic coating was seen in this patient. In the patient treated with colchicine alone, SU levels remained >8 mg/dl, and no sonographic change was observed. In our patients, sonographic signs of deposition of MSU crystals on the surface of hyaline cartilage disappeared completely if sustained normouricemia was achieved. This is the first report showing that characteristic sonographic changes are influenced by ULDs once SU levels remain studies are needed to further assess these potentially important findings.

  16. 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

  17. Rapid growth of ZnO hexagonal prism crystals by direct microwave heating

    Institute of Scientific and Technical Information of China (English)

    ZHU Zhenqi; ZHOU Jian; LIU Guizhen; REN Zhiguo

    2008-01-01

    ZnO hexagonal prism crystals were synthesized from ZnO powders by microwave heating in a short time (within 20 min) without any metal catalyst or transport agent.Zinc oxide raw materials were made by evaporating from the high-temperature zone in an enclosure atmosphere and crystals were grown on the self-source substrate.The inherent asymmetry in microwave heating provides the temperature gradient for crystal growth.Substrate and temperature distribution in the oven show significant effects on the growth of the ZnO crystal.The morphologies demonstrate that these samples are pure hexagonal prism crystals with maximum 80 μm in diameter and 600 μm in length,which possess a well faceted end and side surface.X-ray diffraction (XRD) reveals that these samples are pure crystals.The photoluminescence (PL) exhibits strong ultraviolet emission at room temperature,indicating potential applications for short-wave light-emitting photonic devices.

  18. Quantitative in-situ TEM nanotensile testing of single crystal Ni facilitated by a new sample preparation approach.

    Science.gov (United States)

    Samaeeaghmiyoni, Vahid; Idrissi, Hosni; Groten, Jonas; Schwaiger, Ruth; Schryvers, Dominique

    2017-03-01

    Twin-jet electro-polishing and Focused Ion Beam (FIB) were combined to produce small size Nickel single crystal specimens for quantitative in-situ nanotensile experiments in the transmission electron microscope. The combination of these techniques allows producing samples with nearly defect-free zones in the centre in contrast to conventional FIB-prepared samples. Since TEM investigations can be performed on the electro-polished samples prior to in-situ TEM straining, specimens with desired crystallographic orientation and initial microstructure can be prepared. The present results reveal a dislocation nucleation-controlled plasticity, in which small loops induced by FIB near the edges of the samples play a central role. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Negative refraction at infrared wavelengths in a two-dimensional photonic crystal

    International Nuclear Information System (INIS)

    Berrier, A.; Mulot, M.; Swillo, M.; Qiu, M.; Thylen, L.; Anand, S.; Talneau, A.

    2004-01-01

    We report on the first experimental evidence of negative refraction at telecommunication wavelengths by a two-dimensional photonic crystal field. Samples were fabricated by chemically assisted ion beam etching in the InP-based low-index constrast system. Experiments of beam imaging and light collection show light focusing by the photonic crystal field. Finite-difference time-domain simulations confirm that the observed focusing is due to negative refraction in the photonic crystal area

  20. submitter Light Extraction From Scintillating Crystals Enhanced by Photonic Crystal Structures Patterned by Focused Ion Beam

    CERN Document Server

    Modrzynski, Pawel; Knapitsch, Arno; Kunicki, Piotr; Lecoq, Paul; Moczala, Magdalena; Papakonstantinou, Ioannis; Auffray, Etiennette

    2016-01-01

    “Photonic Crystals (PhC)” have been used in a variety of fields as a structure for improving the light extraction efficiency from materials with high index of refraction. In previous work we already showed the light extraction improvement of several PhC covered LYSO crystals in computer simulations and practical measurements. In this work, new samples are made using different materials and techniques which allows further efficiency improvements. For rapid prototyping of PhC patterns on scintillators we tested a new method using “Focused Ion Beam (FIB)” patterning. The FIB machine is a device similar to a “Scanning Electron Microscope (SEM)”, but it uses ions (mainly gallium) instead of electrons for the imaging of the samples' surface. The additional feature of FIB devices is the option of surface patterning in nano-scale which was exploited for our samples. Three samples using FIB patterning have been produced. One of them is a direct patterning of the extraction face of a 0.8×0.8×10 $mm^3$ LYS...

  1. Crystallization mechanisms of acicular crystals

    Science.gov (United States)

    Puel, François; Verdurand, Elodie; Taulelle, Pascal; Bebon, Christine; Colson, Didier; Klein, Jean-Paul; Veesler, Stéphane

    2008-01-01

    In this contribution, we present an experimental investigation of the growth of four different organic molecules produced at industrial scale with a view to understand the crystallization mechanism of acicular or needle-like crystals. For all organic crystals studied in this article, layer-by-layer growth of the lateral faces is very slow and clear, as soon as the supersaturation is high enough, there is competition between growth and surface-activated secondary nucleation. This gives rise to pseudo-twinned crystals composed of several needle individuals aligned along a crystallographic axis; this is explained by regular over- and inter-growths as in the case of twinning. And when supersaturation is even higher, nucleation is fast and random. In an industrial continuous crystallization, the rapid growth of needle-like crystals is to be avoided as it leads to fragile crystals or needles, which can be partly broken or totally detached from the parent crystals especially along structural anisotropic axis corresponding to weaker chemical bonds, thus leading to slower growing faces. When an activated mechanism is involved such as a secondary surface nucleation, it is no longer possible to obtain a steady state. Therefore, the crystal number, size and habit vary significantly with time, leading to troubles in the downstream processing operations and to modifications of the final solid-specific properties. These results provide valuable information on the unique crystallization mechanisms of acicular crystals, and show that it is important to know these threshold and critical values when running a crystallizer in order to obtain easy-to-handle crystals.

  2. Ptychographic x-ray imaging of surfaces on crystal truncation rod

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Chenhui; Barbour, Andi; Liu, Yaohua; You, Hoydoo, E-mail: hyou@anl.gov [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Harder, Ross; Xu, Ruqing [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Diaz, Ana; Menzel, Andreas [Paul Scherrer Institut, Villigen PSI 5232 (Switzerland); Komanicky, Vladimir [Faculty of Sciences, Safarik University, Kosice 04154 (Slovakia); Huang, Xiaojing [National Synchrotron Light Source II, Brookhaven National Laboratory, Upton, New York 11973 (United States); Pierce, Michael S. [School of Physics and Astronomy, Rochester Institute of Technology, Rochester, New York 14623 (United States)

    2015-03-09

    Ptychography is a high-resolution imaging technique, which does not require lenses for image magnification and which provides phase contrast with high sensitivity. Here, we propose to use x-ray ptychography for the imaging of surface structure in crystalline samples. We show that ptychography can be used to image atomic step structures using coherent diffraction patterns recorded along the crystal truncation rod of a crystal surface. In a proof-of-concept experiment on a Pt (111) sample, we present ptychographic reconstructions showing features consistent with surface steps. Due to the penetration power of x-rays, this method could find interesting applications for the study of surface structures under buried interfaces or in harsh environments.

  3. Ptychographic x-ray imaging of surfaces on crystal truncation rod

    International Nuclear Information System (INIS)

    Zhu, Chenhui; Barbour, Andi; Liu, Yaohua; You, Hoydoo; Harder, Ross; Xu, Ruqing; Diaz, Ana; Menzel, Andreas; Komanicky, Vladimir; Huang, Xiaojing; Pierce, Michael S.

    2015-01-01

    Ptychography is a high-resolution imaging technique, which does not require lenses for image magnification and which provides phase contrast with high sensitivity. Here, we propose to use x-ray ptychography for the imaging of surface structure in crystalline samples. We show that ptychography can be used to image atomic step structures using coherent diffraction patterns recorded along the crystal truncation rod of a crystal surface. In a proof-of-concept experiment on a Pt (111) sample, we present ptychographic reconstructions showing features consistent with surface steps. Due to the penetration power of x-rays, this method could find interesting applications for the study of surface structures under buried interfaces or in harsh environments

  4. Studies on sampling and homogeneous dual readout calorimetry with meta-crystals

    CERN Document Server

    Mavromanolakis, G; Lecoq, P

    2011-01-01

    The meta-crystals concept is an approach that consists of using both undoped and properly doped heavy crystal fibers of identical material as the active medium of a calorimeter. The undoped fibers behave as Cherenkov radiators while the doped ones behave as scintillators. A dual readout calorimeter can be built with its sensitive volume composed of a mixture of both types of crystals. In addition if the calorimeter is adequately finely segmented it can also function as a particle flow calorimeter at the same time. In this way one could possibly combine the advantages of both the particle flow concept and the dual readout scheme. We discuss the approach of dual readout calorimetry with meta-crystals made of Lutetium Aluminium Garnet (LuAG). We brie fly present studies on the material development and first testbeam activities and then focus on performance expectation studies based on simulation. We discuss in more detail the results from generic systematic scannings of the design parameters of a dual readout ca...

  5. 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

  6. 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.

  7. Isolation of a 250 million-year-old halotolerant bacterium from a primary salt crystal

    Science.gov (United States)

    Vreeland, Russell H.; Rosenzweig, William D.; Powers, Dennis W.

    2000-10-01

    Bacteria have been found associated with a variety of ancient samples, however few studies are generally accepted due to questions about sample quality and contamination. When Cano and Borucki isolated a strain of Bacillus sphaericus from an extinct bee trapped in 25-30 million-year-old amber, careful sample selection and stringent sterilization techniques were the keys to acceptance. Here we report the isolation and growth of a previously unrecognized spore-forming bacterium (Bacillus species, designated 2-9-3) from a brine inclusion within a 250million-year-old salt crystal from the Permian Salado Formation. Complete gene sequences of the 16S ribosomal DNA show that the organism is part of the lineage of Bacillus marismortui and Virgibacillus pantothenticus. Delicate crystal structures and sedimentary features indicate the salt has not recrystallized since formation. Samples were rejected if brine inclusions showed physical signs of possible contamination. Surfaces of salt crystal samples were sterilized with strong alkali and acid before extracting brines from inclusions. Sterilization procedures reduce the probability of contamination to less than 1 in 10 9.

  8. Photonic time crystals.

    Science.gov (United States)

    Zeng, Lunwu; Xu, Jin; Wang, Chengen; Zhang, Jianhua; Zhao, Yuting; Zeng, Jing; Song, Runxia

    2017-12-07

    When space (time) translation symmetry is spontaneously broken, the space crystal (time crystal) forms; when permittivity and permeability periodically vary with space (time), the photonic crystal (photonic time crystal) forms. We proposed the concept of photonic time crystal and rewritten the Maxwell's equations. Utilizing Finite Difference Time Domain (FDTD) method, we simulated electromagnetic wave propagation in photonic time crystal and photonic space-time crystal, the simulation results show that more intensive scatter fields can obtained in photonic time crystal and photonic space-time crystal.

  9. Nickel-induced crystallization of amorphous silicon

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, J A; Arce, R D; Buitrago, R H [INTEC (CONICET-UNL), Gueemes 3450, S3000GLN Santa Fe (Argentina); Budini, N; Rinaldi, P, E-mail: jschmidt@intec.unl.edu.a [FIQ - UNL, Santiago del Estero 2829, S3000AOM Santa Fe (Argentina)

    2009-05-01

    The nickel-induced crystallization of hydrogenated amorphous silicon (a-Si:H) is used to obtain large grained polycrystalline silicon thin films on glass substrates. a-Si:H is deposited by plasma enhanced chemical vapour deposition at 200 deg. C, preparing intrinsic and slightly p-doped samples. Each sample was divided in several pieces, over which increasing Ni concentrations were sputtered. Two crystallization methods are compared, conventional furnace annealing (CFA) and rapid thermal annealing (RTA). The crystallization was followed by optical microscopy and scanning electron microscopy observations, X-ray diffraction, and reflectance measurements in the UV region. The large grain sizes obtained - larger than 100{mu}m for the samples crystallized by CFA - are very encouraging for the preparation of low-cost thin film polycrystalline silicon solar cells.

  10. HOLOGRAPHIC GRATING RECORDING IN “LYOTROPIC LIQUID CRYSTAL – VIOLOGEN” SYSTEM

    Directory of Open Access Journals (Sweden)

    Hanna Bordyuh

    2013-12-01

    Full Text Available This work presents the results of nonlinear optical experiment run on the samples of lyotropic liquid crystal (LLC with viologen admixtures. During the experiment we obtained dynamic grating recording on bilayered LLC-viologen samples and determined main characteristics of recoded gratings. It was found out that the recording takes place in a thin near-cathode coloured viologen layer. The analysis of kinetics of thermal gratings erasing showed that contribution of a thermal nonlinearity into general diffraction efficiency is negligible small. The last fact is connected with a separation of LLC-viologen samples under the action of an electric field and heat sink into the liquid crystal layer

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

    Science.gov (United States)

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

    2001-01-01

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

  12. 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.

  13. Highly reproducible alkali metal doping system for organic crystals through enhanced diffusion of alkali metal by secondary thermal activation.

    Science.gov (United States)

    Lee, Jinho; Park, Chibeom; Song, Intek; Koo, Jin Young; Yoon, Taekyung; Kim, Jun Sung; Choi, Hee Cheul

    2018-05-16

    In this paper, we report an efficient alkali metal doping system for organic single crystals. Our system employs an enhanced diffusion method for the introduction of alkali metal into organic single crystals by controlling the sample temperature to induce secondary thermal activation. Using this system, we achieved intercalation of potassium into picene single crystals with closed packed crystal structures. Using optical microscopy and Raman spectroscopy, we confirmed that the resulting samples were uniformly doped and became K 2 picene single crystal, while only parts of the crystal are doped and transformed into K 2 picene without secondary thermal activation. Moreover, using a customized electrical measurement system, the insulator-to-semiconductor transition of picene single crystals upon doping was confirmed by in situ electrical conductivity and ex situ temperature-dependent resistivity measurements. X-ray diffraction studies showed that potassium atoms were intercalated between molecular layers of picene, and doped samples did not show any KH- nor KOH-related peaks, indicating that picene molecules are retained without structural decomposition. During recent decades, tremendous efforts have been exerted to develop high-performance organic semiconductors and superconductors, whereas as little attention has been devoted to doped organic crystals. Our method will enable efficient alkali metal doping of organic crystals and will be a resource for future systematic studies on the electrical property changes of these organic crystals upon doping.

  14. Ensemble refinement shows conformational flexibility in crystal structures of human complement factor D

    International Nuclear Information System (INIS)

    Forneris, Federico; Burnley, B. Tom; Gros, Piet

    2014-01-01

    Ensemble-refinement analysis of native and mutant factor D (FD) crystal structures indicates a dynamical transition in FD from a self-inhibited inactive conformation to a substrate-bound active conformation that is reminiscent of the allostery in thrombin. Comparison with previously observed dynamics in thrombin using NMR data supports the crystallographic ensembles. Human factor D (FD) is a self-inhibited thrombin-like serine proteinase that is critical for amplification of the complement immune response. FD is activated by its substrate through interactions outside the active site. The substrate-binding, or ‘exosite’, region displays a well defined and rigid conformation in FD. In contrast, remarkable flexibility is observed in thrombin and related proteinases, in which Na + and ligand binding is implied in allosteric regulation of enzymatic activity through protein dynamics. Here, ensemble refinement (ER) of FD and thrombin crystal structures is used to evaluate structure and dynamics simultaneously. A comparison with previously published NMR data for thrombin supports the ER analysis. The R202A FD variant has enhanced activity towards artificial peptides and simultaneously displays active and inactive conformations of the active site. ER revealed pronounced disorder in the exosite loops for this FD variant, reminiscent of thrombin in the absence of the stabilizing Na + ion. These data indicate that FD exhibits conformational dynamics like thrombin, but unlike in thrombin a mechanism has evolved in FD that locks the unbound native state into an ordered inactive conformation via the self-inhibitory loop. Thus, ensemble refinement of X-ray crystal structures may represent an approach alternative to spectroscopy to explore protein dynamics in atomic detail

  15. Crystallization in Pd40Ni40P20 glass

    DEFF Research Database (Denmark)

    Jiang, Jianzhong; Saksl, K.; Nishiyama, N.

    2002-01-01

    Phase segregation and the effect of pressure on crystallization of bulk and ribbon Pd40Ni40P20 glasses have been studied by means of differential scanning calorimetry (DSC) and x-ray diffraction. The DSC measurements show only one glass transition event in the samples annealed at different...... temperatures in the supercooled liquid region. Phase analyses reveal at least five crystalline phases crystallized from the glass: monoclinic; body-centered tetragonal; orthorhombic; Ni2Pd2P and fcc-(Ni,Pd) solid solution phases. In the pressure range from 0 to 4.2 GPa, the crystallization temperature...... increases with pressure having a slope of 11 K/GPa. The eutectic crystallization reaction mode and crystalline phases formed are unchanged in the pressure range used. The enhancement of the crystallization temperature with increasing pressure in the glass can be explained by the suppression of atomic...

  16. Crystal plasticity study of single crystal tungsten by indentation tests

    International Nuclear Information System (INIS)

    Yao, Weizhi

    2012-01-01

    Owing to its favorable material properties, tungsten (W) has been studied as a plasma-facing material in fusion reactors. Experiments on W heating in plasma sources and electron beam facilities have shown an intense micro-crack formation at the heated surface and sub-surface. The cracks go deep inside the irradiated sample, and often large distorted areas caused by local plastic deformation are present around the cracks. To interpret the crack-induced microscopic damage evolution process in W, one needs firstly to understand its plasticity on a single grain level, which is referred to as crystal plasticity. In this thesis, the crystal plasticity of single crystal tungsten (SCW) has been studied by spherical and Berkovich indentation tests and the finite element method with a crystal plasticity model. Appropriate values of the material parameters included in the crystal plasticity model are determined by fitting measured load-displacement curves and pile-up profiles with simulated counterparts for spherical indentation. The numerical simulations reveal excellent agreement with experiment. While the load-displacement curves and the deduced indentation hardness exhibit little sensitivity to the indented plane at small indentation depths, the orientation of slip directions within the crystals governs the development of deformation hillocks at the surface. It is found that several factors like friction, indentation depth, active slip systems, misoriented crystal orientation, misoriented sample surface and azimuthal orientation of the indenter can affect the indentation behavior of SCW. The Berkovich indentation test was also used to study the crystal plasticity of SCW after deuterium irradiation. The critical load (pop-in load) for triggering plastic deformation under the indenter is found to depend on the crystallographic orientation. The pop-in loads decrease dramatically after deuterium plasma irradiation for all three investigated crystallographic planes.

  17. Simvastatin-nicotinamide co-crystal: design, preparation and ...

    African Journals Online (AJOL)

    Methods: In silico molecular modeling of Nic counter to SV were investigated using ... Results: In silico results showed that the interaction of Nic with SV took place through ... Conclusion: Co-crystallization using Nic has the potential to enhance drug ... directed to convert the ligand protein data bank ... after each sampling.

  18. Influence of crystal habit on trimethoprim suspension formulation.

    Science.gov (United States)

    Tiwary, A K; Panpalia, G M

    1999-02-01

    The role of crystal habit in influencing the physical stability and pharmacokinetics of trimethoprim suspensions was examined. Different habits for trimethoprim (TMP) were obtained by recrystallizing the commercial sample (PD) utilizing solvent-change precipitation method. Four distinct habits (microscopic observation) belonging to the same polymorphic state (DSC studies) were selected for studies. Preformulation and formulation studies were carried out on suspension dosage forms containing these crystals. The freshly prepared suspensions were also evaluated for their pharmacokinetic behaviour on healthy human volunteers using a cross over study. Variation of crystallization conditions produces different habits of TMP. Among the different crystal habits exhibiting same polymorphic state, the most anisometric crystal showed best physical stability in terms of sedimentation volume and redispersibility. However, habit did not significantly affect the extent of TMP excreted in urine. Modification of surface morphology without significantly altering the polymorphic state can be utilized for improving physical stability of TMP suspensions. However, the pharmacokinetic profile remains unaltered.

  19. Purification, crystallization and preliminary X-ray diffraction studies of parakeet (Psittacula krameri) haemoglobin.

    Science.gov (United States)

    Jaimohan, S M; Naresh, M D; Arumugam, V; Mandal, A B

    2009-10-01

    Birds often show efficient oxygen management in order to meet the special demands of their metabolism. However, the structural studies of avian haemoglobins (Hbs) are inadequate for complete understanding of the mechanism involved. Towards this end, purification, crystallization and preliminary X-ray diffraction studies have been carried out for parakeet Hb. Parakeet Hb was crystallized as the met form in low-salt buffered conditions after extracting haemoglobin from crude blood by microcentrifugation and purifying the sample by column chromatography. Good-quality crystals were grown from 10% PEG 3350 and a crystal diffracted to about 2.8 A resolution. Preliminary diffraction data showed that the Hb crystal belonged to the monoclinic system (space group C2), with unit-cell parameters a = 110.68, b = 64.27, c = 56.40 A, beta = 109.35 degrees . Matthews volume analysis indicated that the crystals contained a half-tetramer in the asymmetric unit.

  20. Dissolution enhancement of Deflazacort using hollow crystals prepared by antisolvent crystallization process.

    Science.gov (United States)

    Paulino, A S; Rauber, G; Campos, C E M; Maurício, M H P; de Avillez, R R; Capobianco, G; Cardoso, S G; Cuffini, S L

    2013-05-13

    Deflazacort (DFZ), a derivate of prednisolone, is a poorly soluble drug which has been proposed to have major advantages over other corticosteroids. Poorly soluble drugs present limited bioavailability due to their low solubility and dissolution rate and several strategies have been developed in order to find ways to improve them. In general, pharmaceutical laboratories use a micronized process to reduce the particle size in order to increase the dissolution of the drugs. However, this process causes changes such as polymorphic transitions, particle agglomeration and a reduction in fluidity and wettability. These solid-state properties affect the dissolution behavior and stability performance of drugs. Crystallization techniques are widely used in the pharmaceutical industry and antisolvent crystallization has been used to obtain ultrafine particles. In this study, DFZ was investigated in terms of its antisolvent crystallization in different solvents and under various preparation conditions (methanol/water ratio, stirring and evaporation rate, etc.), in order to compare the physicochemical properties between crystallized samples and raw materials available on the Brazilian market with and without micronization. Crystalline structure, morphology, and particle size, and their correlation with the Intrinsic Dissolution Rate (IDR) and dissolution profile as relevant biopharmaceutical properties were studied. Crystallization conditions were achieved which provided crystalline samples of hollow-shaped crystals with internal channels, which increased the dissolution rate of DFZ. The antisolvent crystallization process allowed the formation of hollow crystals, which demonstrated a better dissolution profile than the raw material (crystalline and micronized), making this a promising technique as a crystallization strategy for improving the dissolution and thus the bioavailability of poorly soluble drugs. Copyright © 2013 Elsevier B.V. All rights reserved.

  1. Orientation effect on recovery and recrystallization of cold rolled niobium single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Srinivasan, R. [Center for Accelerated Maturation of Materials, Department of Materials Science and Engineering, Ohio State University, Columbus, OH 43210 (United States)], E-mail: rajagopalan.5@osu.edu; Viswanathan, G.B.; Levit, V.I.; Fraser, H.L. [Center for Accelerated Maturation of Materials, Department of Materials Science and Engineering, Ohio State University, Columbus, OH 43210 (United States)

    2009-05-15

    Single crystal sheets of niobium with initial orientations of (0 0 1) [11-bar0], (1 1 0) [11-bar 0] and (1 1 1) [11-bar0] were rolled at room temperature in the strain range of 25-50%. The deformed specimens were vacuum annealed at temperatures of 800 deg. C, 1000 deg. C, and 1200 deg. C for 3 h. TEM, SEM-OIM and optical microscopy revealed orientation stability in (0 0 1) and (1 1 0) rolled samples with no recrystallization observed after annealing. Samples rolled along (1 1 1) partially recrystallized after annealing at 1000 deg. C and 1200 deg. C. A relatively small increase was observed in hardness of (0 0 1) rolled crystals between 25% and 50% strain, implying low work hardening rates. (1 1 1) rolled samples showed higher hardening rates, and enhanced recovery in hardness values after annealing, due to partial recrystallization. Conditions have been identified for the deformation and annealing of niobium single crystals, enabling the preservation of single crystal structure and near-complete recovery of mechanical properties. A simple crystallographic model is proposed, giving an explanation for the observed orientation stability in (0 0 1) and (1 1 0) rolled samples, and the tendency towards instability and recrystallization in (1 1 1) rolled samples.

  2. Towards 3D crystal orientation reconstruction using automated crystal orientation mapping transmission electron microscopy (ACOM-TEM).

    Science.gov (United States)

    Kobler, Aaron; Kübel, Christian

    2018-01-01

    To relate the internal structure of a volume (crystallite and phase boundaries) to properties (electrical, magnetic, mechanical, thermal), a full 3D reconstruction in combination with in situ testing is desirable. In situ testing allows the crystallographic changes in a material to be followed by tracking and comparing the individual crystals and phases. Standard transmission electron microscopy (TEM) delivers a projection image through the 3D volume of an electron-transparent TEM sample lamella. Only with the help of a dedicated TEM tomography sample holder is an accurate 3D reconstruction of the TEM lamella currently possible. 2D crystal orientation mapping has become a standard method for crystal orientation and phase determination while 3D crystal orientation mapping have been reported only a few times. The combination of in situ testing with 3D crystal orientation mapping remains a challenge in terms of stability and accuracy. Here, we outline a method to 3D reconstruct the crystal orientation from a superimposed diffraction pattern of overlapping crystals without sample tilt. Avoiding the typically required tilt series for 3D reconstruction enables not only faster in situ tests but also opens the possibility for more stable and more accurate in situ mechanical testing. The approach laid out here should serve as an inspiration for further research and does not make a claim to be complete.

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

    International Nuclear Information System (INIS)

    Wu, Y.Q.; Huang, F.L.

    2010-01-01

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

  4. Purification, crystallization and preliminary X-ray diffraction studies of parakeet (Psittacula krameri) haemoglobin

    International Nuclear Information System (INIS)

    Jaimohan, S. M.; Naresh, M. D.; Arumugam, V.; Mandal, A. B.

    2009-01-01

    Parakeet (Psittacula krameri) haemoglobin has been purified and crystallized under low salt buffered conditions. Preliminary analysis of the crystal that belonged to monoclinic system (C2) is reported. Birds often show efficient oxygen management in order to meet the special demands of their metabolism. However, the structural studies of avian haemoglobins (Hbs) are inadequate for complete understanding of the mechanism involved. Towards this end, purification, crystallization and preliminary X-ray diffraction studies have been carried out for parakeet Hb. Parakeet Hb was crystallized as the met form in low-salt buffered conditions after extracting haemoglobin from crude blood by microcentrifugation and purifying the sample by column chromatography. Good-quality crystals were grown from 10% PEG 3350 and a crystal diffracted to about 2.8 Å resolution. Preliminary diffraction data showed that the Hb crystal belonged to the monoclinic system (space group C2), with unit-cell parameters a = 110.68, b = 64.27, c = 56.40 Å, β = 109.35°. Matthews volume analysis indicated that the crystals contained a half-tetramer in the asymmetric unit

  5. Growth of single crystals of BaFe12O19 by solid state crystal growth

    International Nuclear Information System (INIS)

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

    2016-01-01

    Single crystals of BaFe 12 O 19 are grown for the first time by solid state crystal growth. Seed crystals of BaFe 12 O 19 are buried in BaFe 12 O 19 +1 wt% BaCO 3 powder, which are then pressed into pellets containing the seed crystals. During sintering, single crystals of BaFe 12 O 19 up to ∼130 μm thick in the c-axis direction grow on the seed crystals by consuming grains from the surrounding polycrystalline matrix. Scanning electron microscopy-energy dispersive spectroscopy analysis shows that the single crystal and the surrounding polycrystalline matrix have the same chemical composition. Micro-Raman scattering shows the single crystal to have the BaFe 12 O 19 structure. The optimum growth temperature is found to be 1200 °C. The single crystal growth behavior is explained using the mixed control theory of grain growth. - Highlights: • Single crystals of BaFe 12 O 19 are grown by solid state crystal growth. • A single crystal up to ∼130 μm thick (c-axis direction) grows on the seed crystal. • The single crystal and surrounding ceramic matrix have similar composition. • Micro-Raman scattering shows the single crystal has the BaFe 12 O 19 structure.

  6. Crystal Systems.

    Science.gov (United States)

    Schomaker, Verner; Lingafelter, E. C.

    1985-01-01

    Discusses characteristics of crystal systems, comparing (in table format) crystal systems with lattice types, number of restrictions, nature of the restrictions, and other lattices that can accidently show the same metrical symmetry. (JN)

  7. Crystallization behavior of Ge-doped eutectic Sb70Te30 films in optical disks

    International Nuclear Information System (INIS)

    Khulbe, Pramod K.; Hurst, Terril; Mansuripur, Masud; Horie, Michikazu

    2002-01-01

    We report laser-induced crystallization behavior of binary Sb-Te and ternary Ge-doped eutectic Sb70Te30 thin film samples in a typical quadrilayer stack as used in phase-change optical disk data storage. Several experiments have been conducted on a two-laser static tester in which one laser operating in pulse mode writes crystalline marks on amorphous film or amorphous marks on crystalline film, while the second laser operating at low-power cw mode simultaneously monitors the progress of the crystalline or amorphous mark formation in real time in terms of the reflectivity variation. The results of this study show that the crystallization kinetics of this class of film is strongly growth dominant, which is significantly different from the crystallization kinetics of stochiometric Ge-Sb-Te compositions. In Sb-Te and Ge-doped eutectic Sb70Te30 thin-film samples, the crystallization behavior of the two forms of amorphous states, namely, as-deposited amorphous state and melt-quenched amorphous state, remains approximately same. We have also presented experiments showing the effect of the variation of the Sb/Te ratio and Ge doping on the crystallization behavior of these films

  8. NMR of bicelles: orientation and mosaic spread of the liquid-crystal director under sample rotation

    International Nuclear Information System (INIS)

    Zandomeneghi, Giorgia; Tomaselli, Marco; Williamson, Philip T.F.; Meier, Beat H.

    2003-01-01

    Model-membrane systems composed of liquid-crystalline bicellar phases can be uniaxially oriented with respect to a magnetic field, thereby facilitating structural and dynamics studies of membrane-associated proteins. Here we quantitatively characterize a method that allows the manipulation of the direction of this uniaxial orientation. Bicelles formed from DMPC/DHPC are examined by 31 P NMR under variable-angle sample-spinning (VAS) conditions, confirming that the orientation of the liquid-crystalline director can be influenced by sample spinning. The director is perpendicular to the rotation axis when Θ (the angle between the sample-spinning axis and the magnetic field direction) is smaller than the magic angle, and is parallel to the rotation axis when Θ is larger than the magic angle. The new 31 P NMR VAS data presented are considerably more sensitive to the orientation of the bicelle than earlier 2 H studies and the analysis of the sideband pattern allows the determination of the orientation of the liquid-crystal director and its variation over the sample, i.e., the mosaic spread. Under VAS, the mosaic spread is small if Θ deviates significantly from the magic angle but becomes very large at the magic angle

  9. Crystals and tablets in the Spanish ecstasy market 2000-2014: Are they the same or different in terms of purity and adulteration?

    Science.gov (United States)

    Vidal Giné, Claudio; Ventura Vilamala, Mireia; Fornís Espinosa, Iván; Gil Lladanosa, Cristina; Calzada Álvarez, Nú; Fitó Fruitós, Ariadna; Rodríguez Rodríguez, Joan; Domíngo Salvany, Antonia; de la Torre Fornell, Rafael

    2016-06-01

    Although 3,4-methylenedioxymethamphetamine (MDMA) has a long history in recreational settings, research on its composition (purity and adulteration) has focused only on tablets even though crystal format is readily available for users. Drug specimens collected between January 2000 and December 2014 were analyzed at Energy Control's facilities. All samples were voluntarily provided by drug users. Sample identification was made with thin layer chromatography and gas chromatography coupled to mass spectrometry, and quantification with ultraviolet spectrophotometry (only in unadulterated samples). Between January 2000 and December 2014, 6200 samples purchased as ecstasy by their users were analyzed. Crystals were the most frequent format (60.6%) followed by tablets (38.8%). During the study period, the proportion of samples containing only MDMA was higher in crystals than in tablets. Compared with tablets, adulterated crystal samples contained the same number of adulterants but more combinations of different substances. Although caffeine was commonly detected as adulterant both in crystals and tablets, other substances such as phenacetin, lidocaine, dextrometorphan or methamphetamine were detected almost exclusively in crystal samples. The amount of MDMA in crystal samples remained stable unlike tablets for which a huge increase in MDMA dose was observed since 2010. Crystal samples of ecstasy showed clear differences compared to ecstasy tablets and this must be taken into account both in research and harm reduction. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  10. Fracture mechanics of hydroxyapatite single crystals under geometric confinement.

    Science.gov (United States)

    Libonati, Flavia; Nair, Arun K; Vergani, Laura; Buehler, Markus J

    2013-04-01

    Geometric confinement to the nanoscale, a concept that refers to the characteristic dimensions of structural features of materials at this length scale, has been shown to control the mechanical behavior of many biological materials or their building blocks, and such effects have also been suggested to play a crucial role in enhancing the strength and toughness of bone. Here we study the effect of geometric confinement on the fracture mechanism of hydroxyapatite (HAP) crystals that form the mineralized phase in bone. We report a series of molecular simulations of HAP crystals with an edge crack on the (001) plane under tensile loading, and we systematically vary the sample height whilst keeping the sample and the crack length constant. We find that by decreasing the sample height the stress concentration at the tip of the crack disappears for samples with a height smaller than 4.15nm, below which the material shows a different failure mode characterized by a more ductile mechanism with much larger failure strains, and the strength approaching that of a flaw-less crystal. This study directly confirms an earlier suggestion of a flaw-tolerant state that appears under geometric confinement and may explain the mechanical stability of the reinforcing HAP platelets in bone. Copyright © 2012 Elsevier Ltd. All rights reserved.

  11. Effect of Nickel sulphate on Growth, Structural, Optical, Mechanical and thermal properties of L-alanine Single Crystals (LANS)

    Science.gov (United States)

    Jothimani, R.; Selvarajan, P.

    2017-08-01

    The nonlinear optical materials find excellent place in frequency conversion, optical telecommunication, image processing, optical computing, and data storage. Due to possessing chiral symmetry and nature of crystallize in noncentro-symmetric space groups, the amino acids are applicable in NLO applications. A transparent nickel sulphate admixtured L-alanine crystal has been developed by solution method. X ray diffraction analysis depicts the orthorhombic crystal system of the sample. NLO efficiency of the sample was found to be highly pronounced compare to KDP. An enhanced linear optical property of the sample shows its suitability for NLO applications. Thermal behaviour of the sample was found by TGA/DTA analysis. Hardness parameters were also found for the sample by microhardness measurements. Laser damage threshold were also measured using Nd: YAG laser.

  12. Crystallization peculiarities in metallic glasses

    International Nuclear Information System (INIS)

    Serebryakov, A.V.; Abrosimova, G.E.; Aronin, A.S.

    1985-01-01

    Methods of X-ray electron microscopy and X-ray diffraction analysis were used to investigate the peculiarities of crystallization of amorphous metallic Fe-B and Fe-Si-B alloys related to sufficient change of volume when passing from amorphous to crystalline state and the effect of sample prehistory on its thermal stability and crystallization kinetics. The dependence of morphology of crystalline phases formed during crystallization of amorphous Fe-B alloys on sample thickness was revealed and investigated. The model explaining this dependence was suggested. The observed differences are related, according to the model, with different diffusion ways of ''poles'' - elementary carriers of empty volume to their sinks

  13. Defined PEG smears as an alternative approach to enhance the search for crystallization conditions and crystal-quality improvement in reduced screens

    Energy Technology Data Exchange (ETDEWEB)

    Chaikuad, Apirat, E-mail: apirat.chaikuad@sgc.ox.ac.uk [University of Oxford, Old Road Campus Research Building, Roosevelt Drive, Headington, Oxford OX3 7DQ (United Kingdom); Knapp, Stefan [University of Oxford, Old Road Campus Research Building, Roosevelt Drive, Headington, Oxford OX3 7DQ (United Kingdom); Johann Wolfgang Goethe-University, Building N240 Room 3.03, Max-von-Laue-Strasse 9, 60438 Frankfurt am Main (Germany); Delft, Frank von, E-mail: apirat.chaikuad@sgc.ox.ac.uk [University of Oxford, Old Road Campus Research Building, Roosevelt Drive, Headington, Oxford OX3 7DQ (United Kingdom)

    2015-07-28

    An alternative strategy for PEG sampling is suggested through the use of four newly defined PEG smears to enhance chemical space in reduced screens with a benefit towards protein crystallization. The quest for an optimal limited set of effective crystallization conditions remains a challenge in macromolecular crystallography, an issue that is complicated by the large number of chemicals which have been deemed to be suitable for promoting crystal growth. The lack of rational approaches towards the selection of successful chemical space and representative combinations has led to significant overlapping conditions, which are currently present in a multitude of commercially available crystallization screens. Here, an alternative approach to the sampling of widely used PEG precipitants is suggested through the use of PEG smears, which are mixtures of different PEGs with a requirement of either neutral or cooperatively positive effects of each component on crystal growth. Four newly defined smears were classified by molecular-weight groups and enabled the preservation of specific properties related to different polymer sizes. These smears not only allowed a wide coverage of properties of these polymers, but also reduced PEG variables, enabling greater sampling of other parameters such as buffers and additives. The efficiency of the smear-based screens was evaluated on more than 220 diverse recombinant human proteins, which overall revealed a good initial crystallization success rate of nearly 50%. In addition, in several cases successful crystallizations were only obtained using PEG smears, while various commercial screens failed to yield crystals. The defined smears therefore offer an alternative approach towards PEG sampling, which will benefit the design of crystallization screens sampling a wide chemical space of this key precipitant.

  14. Control of nucleation and crystal growth of a silicate apatitic phase in a glassy matrix

    International Nuclear Information System (INIS)

    Ligny, D.; Caurant, D.; Bardez, I.; Dussossoy, J.L.; Loiseau, P.; Neuville, D.R.

    2004-01-01

    Nucleation and growth of crystal in an oxide glass was studied in a Si B Al Zr Nd Ca Na O system. The nucleation and growth process were monitored by thermal analysis and isothermal experiments. The effect of the network modifier was studied. Therefore for a Ca rich sample the crystallization is homogeneous in the bulk showing a slow increase of crystallinity as temperature increases. On the other hand, a Na rich sample undergoes several crystallization processes in the bulk or from the surface, leading to bigger crystals. The activation energy of the viscous flow and the glass transition are of same magnitude when that of crystallization is a lot smaller. Early diffusion of element is done with a mechanism different than the configurational rearrangements of the liquid sate. The global density and small size of the crystals within the Ca rich matrix confirmed that it would be a profitable waste form for minor actinides. (authors)

  15. Order-parameter-aided temperature-accelerated sampling for the exploration of crystal polymorphism and solid-liquid phase transitions

    International Nuclear Information System (INIS)

    Yu, Tang-Qing; Vanden-Eijnden, Eric; Chen, Pei-Yang; Chen, Ming; Samanta, Amit; Tuckerman, Mark

    2014-01-01

    The problem of predicting polymorphism in atomic and molecular crystals constitutes a significant challenge both experimentally and theoretically. From the theoretical viewpoint, polymorphism prediction falls into the general class of problems characterized by an underlying rough energy landscape, and consequently, free energy based enhanced sampling approaches can be brought to bear on the problem. In this paper, we build on a scheme previously introduced by two of the authors in which the lengths and angles of the supercell are targeted for enhanced sampling via temperature accelerated adiabatic free energy dynamics [T. Q. Yu and M. E. Tuckerman, Phys. Rev. Lett. 107, 015701 (2011)]. Here, that framework is expanded to include general order parameters that distinguish different crystalline arrangements as target collective variables for enhanced sampling. The resulting free energy surface, being of quite high dimension, is nontrivial to reconstruct, and we discuss one particular strategy for performing the free energy analysis. The method is applied to the study of polymorphism in xenon crystals at high pressure and temperature using the Steinhardt order parameters without and with the supercell included in the set of collective variables. The expected fcc and bcc structures are obtained, and when the supercell parameters are included as collective variables, we also find several new structures, including fcc states with hcp stacking faults. We also apply the new method to the solid-liquid phase transition in copper at 1300 K using the same Steinhardt order parameters. Our method is able to melt and refreeze the system repeatedly, and the free energy profile can be obtained with high efficiency

  16. Mass counting of radioactivity samples

    International Nuclear Information System (INIS)

    Oesterlin, D.L.; Obrycki, R.F.

    1977-01-01

    A method and apparatus for concurrently counting a plurality of radioactive samples is claimed. The position sensitive circuitry of a scintillation camera is employed to sort electrical pulses resulting from scintillations according to the geometrical locations of scintillations causing those pulses. A scintillation means, in the form of a scintillating crystal material or a liquid scintillator, is positioned proximate to an array of radioactive samples. Improvement in the accuracy of pulse classification may be obtained by employing collimating means. If a plurality of scintillation crystals are employed to measure the iodine-125 content of samples, a method and means are provided for correcting for variations in crystal light transmission properties, sample volume, and sample container radiation absorption. 2 claims, 7 drawing figures

  17. Angular distributions of sputtered particles from lithium-implanted aluminium and copper crystals

    International Nuclear Information System (INIS)

    Johansen, A.; Johnson, E.; Sarholt-Kristensen, L.; Steenstrup, S.; Andersen, H.H.; Buhanov, V.M.; Chernysh, V.S.; Ivanov, I.N.; Minnebaev, K.F.

    1991-01-01

    The anisotropy of angular distributions of sputtered ions from lithium implanted aluminium and copper single crystals, measured by SIMS analysis, have been used to obtain information about the microstructure of the implanted layers. Sputtered Al + distributions from the {111} surface show three-fold symmetry with maximum intensity near the and directions respectively, while Li + distributions show maximum intensity only in the directions. From {100} crystals the Al + distributions have four-fold symmetry while there are no preferential ejection directions for the Li + ions. This agrees conceptually with the fact that the implanted layer contains the ordered Al 3 Li (δ') phase, which has earlier been observed by TEM analysis on implanted samples. In contrast, a similar study of Li + implanted copper crystals shows that the implanted lithium is randomly located. (orig.)

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

    Science.gov (United States)

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

    2017-12-01

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

  19. Strong dielectric liquid crystal polymer (Part 3)

    Energy Technology Data Exchange (ETDEWEB)

    Kurata, Hideaki; Shibasaki, Akira

    1988-11-01

    Influence of change of molecular parameters on liquid crystal condition is studied to get the correlation between molecular structure of liquid crystal and phase structure or visco-elastic properties. Eight kinds of biphenyl type liquid crystals with polyacrilate main chain and triphenyl type liquid crystals were used as samples. Followings were found by a ploarizing microscope and X-ray diffraction: Phases are transferred from isotropic phase S/sub A/ phase S/sup *//sub C/ phase S/sub 1/ phase to solid on temperature desending sequence. Degree of polymerization changes only these transfer point but spacer length affects not only transfer points and layer distance but also liquid crystal structure itself. Visco-elasticity of isotropic phase shows Newtonian viscosity and is affected by the main chain length. Macroscopic and microscopic structures influence on viscoelasticity in S/sub A/ phase and S/sup *//sub C/ phase. Two rapid rises of viscoelasticity are found in low molecular weight liquid crystal when S/sub A/ transfer and S/sub A/ to S/sup *//sub C/ transfer occur by temperature desending from the isotropic phase. Viscoelastic behavior is contributed by the properties of domain itself and interaction between domains, and the interaction is changed by polymerization. 6 references, 13 figures, 1 table.

  20. Order-disorder-reorder process in thermally treated dolomite samples: a combined powder and single-crystal X-ray diffraction study

    Science.gov (United States)

    Zucchini, A.; Comodi, P.; Katerinopoulou, A.; Balic-Zunic, T.; McCammon, C.; Frondini, F.

    2012-04-01

    A combined powder and single-crystal X-ray diffraction analysis of dolomite [CaMg(CO3)2] heated to 1,200°C at 3 GPa was made to study the order-disorder-reorder process. The order/disorder transition is inferred to start below 1,100°C, and complete disorder is attained at approximately 1,200°C. Twinned crystals characterized by high internal order were found in samples annealed over 1,100°C, and their fraction was found to increase with temperature. Evidences of twinning domains combined with probable remaining disordered portions of the structure imply that reordering processes occur during the quench. Twin domains are hereby proposed as a witness to thermally induced intra-layer-type cation disordering.

  1. At last! The single-crystal X-ray structure of a naturally occurring sample of the ilmenite-type oxide FeCrO3.

    Science.gov (United States)

    Pérez-Cruz, María Ana; Elizalde-González, María de la Paz; Escudero, Roberto; Bernès, Sylvain; Silva-González, Rutilo; Reyes-Ortega, Yasmi

    2015-10-01

    A natural single crystal of the ferrimagnetic oxide FeCrO3, which was found in an opencast mine situated in the San Luis Potosí State in Mexico, has been characterized in order to elucidate some outstanding issues about the actual structure of this material. The single-crystal X-ray analysis unambiguously shows that transition metal cations are segregated in alternating layers normal to the threefold crystallographic axis, affording a structure isomorphous to that of ilmenite (FeTiO3), in the space group R3̅. The possible occurrence of cation antisite and vacancy defects is below the limit of detection available from X-ray data. Structural and magnetic results are in agreement with the coherent slow intergrowth of magnetic phases provided by the two antiferromagnetic corundum-type parent oxides Fe2O3 (hematite) and Cr2O3 (eskolaite). Our results are consistent with the most recent density functional theory (DFT) studies carried out on digital FeCrO3 [Sadat Nabi & Pentcheva (2011). Phys. Rev. B, 83, 214424], and suggest that synthetic samples of FeCrO3 might present a cation distribution different to that of the ilmenite structural type.

  2. 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.

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

    Science.gov (United States)

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

    2016-06-01

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

  4. Multiple sample, radioactive particle counting apparatus

    International Nuclear Information System (INIS)

    Reddy, R.R.V.; Kelso, D.M.

    1978-01-01

    An apparatus is described for determining the respective radioactive particle sample count being emitted from radioactive particle containing samples. It includes means for modulating the information on the radioactive particles being emitted from the samples, coded detecting means for sequentially detecting different respective coded combinations of the radioactive particles emitted from more than one but less than all of the samples, and processing the modulated information to derive the sample count for each sample. It includes a single light emitting crystal next to a number of samples, an encoder belt sequentially movable between the crystal and the samples. The encoder belt has a coded array of apertures to provide corresponding modulated light pulses from the crystal, and a photomultiplier tube to convert the modulated light pulses to decodable electrical signals for deriving the respective sample count

  5. Liquid nitrogen dewar for protein crystal growth

    Science.gov (United States)

    2001-01-01

    Gaseous Nitrogen Dewar apparatus developed by Dr. Alex McPherson of the University of California, Irvine for use aboard Mir and the International Space Station allows large quantities of protein samples to be crystallized in orbit. The specimens are contained either in plastic tubing (heat-sealed at each end). Biological samples are prepared with a precipitating agent in either a batch or liquid-liquid diffusion configuration. The samples are then flash-frozen in liquid nitrogen before crystallization can start. On orbit, the Dewar is placed in a quiet area of the station and the nitrogen slowly boils off (it is taken up by the environmental control system), allowing the proteins to thaw to begin crystallization. The Dewar is returned to Earth after one to four months on orbit, depending on Shuttle flight opportunities. The tubes then are analyzed for crystal presence and quality

  6. Polarization singularities of optical fields caused by structural dislocations in crystals

    International Nuclear Information System (INIS)

    Savaryn, V; Vasylkiv, Yu; Krupych, O; Skab, I; Vlokh, R

    2013-01-01

    We analyze polarization singularities of optical beams that propagate through crystals possessing structural dislocations. We show that screw dislocations of crystalline structure can lead to the appearance of purely screw-type dislocations of light wavefronts. This can happen only in crystals that belong to trigonal and cubic systems. These polarization singularities will give rise to optical vortices with the topological charge equal to ±1, whenever a crystal sample is placed between crossed circular polarizers. We have also found that edge dislocations present in the cubic and trigonal crystals, with the Burgers vector perpendicular to the three-fold symmetry axes, can impose mixed screw-edge dislocations in the wavefronts of optical beams and generate singly charged optical vortices. The results of our analysis can be applied for detecting and identifying dislocations of different types available in crystals. (paper)

  7. Effect of SHI irradiation on structural, surface morphological and optical studies of CVT grown ZnSSe single crystals

    International Nuclear Information System (INIS)

    Kannappan, P.; Asokan, K.; Krishna, J.B.M.; Dhanasekaran, R.

    2013-01-01

    Highlights: •CVT grown ZnSSe single crystals were irradiated with 120 MeV Au ion. •The GIXRD results show the FWHM increases with increasing ion fluency. •The AFM study show the surface roughness increases with ion fluency. •The optical band gap energy vary with increasing ion fluency. •The PL emission decreases with increasing ion fluency. -- Abstract: The ZnSSe single crystals grown by chemical vapour transport (CVT) method have been irradiated by 120 MeV Au 9+ ions at room temperature with fluences of 1 × 10 12 and 5 × 10 12 ions/cm 2 . The grazing incidence X-ray diffraction (GIXRD) results show that the full width at half maximum (FWHM) value for the as grown ZnSSe crystal is 0.215°; and for the irradiated samples, the FWHM values are 0.413° and 0.625°, with the increase of ion fluences. The atomic force microscopy (AFM) studies reveal the formation of the pits and islands due to irradiation. The optical absorption cut off wavelength is found to be 441 nm for as grown ZnSSe crystal. The cut off values are increased to 447 nm and 457 nm for the irradiated samples with increasing ion fluency. The photoluminescence studies show the emission for the as grown ZnSSe is 590 nm whereas for the irradiated samples in the emission range it is 580–590 nm and 575–595 nm due to SHI irradiation. FT-Raman spectra analysis has been made for the ZnSSe single crystals and irradiated samples. The results are discussed in detail

  8. Effect of SHI irradiation on structural, surface morphological and optical studies of CVT grown ZnSSe single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Kannappan, P. [Crystal Growth Centre, Anna University, Chennai 600 025 (India); Asokan, K. [Inter University Accelerator Centre, Aruna Asaf Ali Marg, New Delhi 110 067 (India); Krishna, J.B.M. [UGC-DAE Consortium for Scientific Research, III-/LB-8, Bidhan nagar, Kolkata 700 098 (India); Dhanasekaran, R., E-mail: rdcgc@yahoo.com [Crystal Growth Centre, Anna University, Chennai 600 025 (India)

    2013-12-15

    Highlights: •CVT grown ZnSSe single crystals were irradiated with 120 MeV Au ion. •The GIXRD results show the FWHM increases with increasing ion fluency. •The AFM study show the surface roughness increases with ion fluency. •The optical band gap energy vary with increasing ion fluency. •The PL emission decreases with increasing ion fluency. -- Abstract: The ZnSSe single crystals grown by chemical vapour transport (CVT) method have been irradiated by 120 MeV Au{sup 9+} ions at room temperature with fluences of 1 × 10{sup 12} and 5 × 10{sup 12} ions/cm{sup 2}. The grazing incidence X-ray diffraction (GIXRD) results show that the full width at half maximum (FWHM) value for the as grown ZnSSe crystal is 0.215°; and for the irradiated samples, the FWHM values are 0.413° and 0.625°, with the increase of ion fluences. The atomic force microscopy (AFM) studies reveal the formation of the pits and islands due to irradiation. The optical absorption cut off wavelength is found to be 441 nm for as grown ZnSSe crystal. The cut off values are increased to 447 nm and 457 nm for the irradiated samples with increasing ion fluency. The photoluminescence studies show the emission for the as grown ZnSSe is 590 nm whereas for the irradiated samples in the emission range it is 580–590 nm and 575–595 nm due to SHI irradiation. FT-Raman spectra analysis has been made for the ZnSSe single crystals and irradiated samples. The results are discussed in detail.

  9. Positron annihilation spectroscopy of vacancy aggregates in neutron-irradiated MgO crystals

    International Nuclear Information System (INIS)

    Pareja, R.; De La Cruz, R.M.; Gonzalez, R.; Chen, Y.; Department of Energy, Washington, DC

    1992-01-01

    Positron annihilation measurements in neutron-irradiated MgO crystals show that the positron lifetime is shorter than in as-grown crystals, suggesting that most of the defects produced by neutron irradiations are positively charged. The concentration of the neutral anion vacancy (possibly also the neutral anion divacancy) is estimated to be no more than ∼ 10 16 cm -3 for samples irradiated to a dose of 10 17 to 10 19 n cm -2 . Annealing experiments on the neutron-irradiated crystals show a significant increase in the positron lifetime after anneals at 900 K. The increase is attributed to positron trapping by anion-vacancy aggregates. A lifetime of (284±15)ps is tentatively assigned to positrons trapped in these aggregates. (Author)

  10. Automation in biological crystallization.

    Science.gov (United States)

    Stewart, Patrick Shaw; Mueller-Dieckmann, Jochen

    2014-06-01

    Crystallization remains the bottleneck in the crystallographic process leading from a gene to a three-dimensional model of the encoded protein or RNA. Automation of the individual steps of a crystallization experiment, from the preparation of crystallization cocktails for initial or optimization screens to the imaging of the experiments, has been the response to address this issue. Today, large high-throughput crystallization facilities, many of them open to the general user community, are capable of setting up thousands of crystallization trials per day. It is thus possible to test multiple constructs of each target for their ability to form crystals on a production-line basis. This has improved success rates and made crystallization much more convenient. High-throughput crystallization, however, cannot relieve users of the task of producing samples of high quality. Moreover, the time gained from eliminating manual preparations must now be invested in the careful evaluation of the increased number of experiments. The latter requires a sophisticated data and laboratory information-management system. A review of the current state of automation at the individual steps of crystallization with specific attention to the automation of optimization is given.

  11. Effect of wheel speed on the crystallization behavior of as-quenched Nd-Fe-B alloys

    Directory of Open Access Journals (Sweden)

    Kuo Men

    2016-02-01

    Full Text Available A series of alloys composed of Nd9Fe85Nb0.5B5.5 were prepared through rapid quenching by different wheel speeds. Nanocomposite was usually obtained by subjecting the as-quenched alloys to a crystallization annealing. The crystallization behavior was investigated by differential scanning calorimetry (DSC as the primary method. The results showed that the DSC curve of sample prepared at 15 m/s had only one exothermic peak at about 690 °C. When the wheel speed increased to 18-27 m/s, one more peak at 590 °C appeared. Moreover, the intensity of this new peak enhances while the original one at 690 °C declined as the speed increases within this range. When the speed further grew up to 30, 35, or 40 m/s , only the peak at 590 °C remained while the other disappeared. This could be ascribed to the different initial phase structures of the alloys, which were found to vary with the wheel speeds. As can be seen, with increasing the wheel speed, the contents of amorphous and metastable phase increased while Nd2Fe14B phase decreased. This change resulted in a huge effect on the crystallization behavior. We could deduce the relative content of each phase from the integral areas of peaks in DSC curves in different samples and figure out the phase transition in the crystallization. The results showed that the crystallization of samples prepared by relatively high speeds, which are almost amorphous initially, manifest as only one step, while those prepared by relatively low speeds showed two. Subsequently, we analyzed the crystallization process and interpreted it from the theory of energy barrier.

  12. Thermoelectric properties and thermal stability of Bi-doped PbTe single crystal

    Science.gov (United States)

    Chen, Zhong; Li, Decong; Deng, Shuping; Tang, Yu; Sun, Luqi; Liu, Wenting; Shen, Lanxian; Yang, Peizhi; Deng, Shukang

    2018-06-01

    In this study, n-type Bi-doped single-crystal PbTe thermoelectric materials were prepared by melting and slow cooling method according to the stoichiometric ratio of Pb:Bi:Te = 1-x:x:1 (x = 0, 0.1, 0.15, 0.2, 0.25). The X-ray diffraction patterns of Pb1-xBixTe samples show that all main diffraction peaks are well matched with the PbTe matrix, which has a face-centered cubic structure with the space group Fm 3 bar m . Electron probe microanalysis reveals that Pb content decreases gradually, and Te content remains invariant basically with the increase of Bi content, indicating that Bi atoms are more likely to replace Pb atoms. Thermal analysis shows that the prepared samples possess relatively high thermal stability. Simultaneously, transmission electron microscopy and selected area electron diffraction pattern indicate that the prepared samples have typical single-crystal structures with good mechanical properties. Moreover, the electrical conductivity of the prepared samples improved significantly compared with that of the pure sample, and the maximum ZT value of 0.84 was obtained at 600 K by the sample with x = 0.2.

  13. PDF analysis on re-crystallized structure from amorphous BiT

    Energy Technology Data Exchange (ETDEWEB)

    Yoneda, Yasuhiro [Japan Atomic Energy Research Institute, Synchrotron Radiation Research Center, Kouto 1-1-1, Mikazuki-cho, Sayo-gun, Hyogo 679-5148 (Japan)]. E-mail: yoneda@spring8.or.jp; Kohara, Shinji [Synchrotron Radiation Research Laboratory, Japan Synchrotron Radiation, Research Institute, Kouto 1-1-1, Mikazuki-cho, Sayo-gun, Hyogo 679-5198 (Japan); Hamazaki, Shin' ichi [Department of Electronics, Iwaki Meisei University, Iino 5-5-1, Chuohdai, Fukushima 970-8551 (Japan); Takashige, Masaaki [Department of Electronics, Iwaki Meisei University, Iino 5-5-1, Chuohdai, Fukushima 970-8551 (Japan); Mizuki, Jun' ichiro [Japan Atomic Energy Research Institute, Synchrotron Radiation Research Center, Kouto 1-1-1, Mikazuki-cho, Sayo-gun, Hyogo 679-5148 (Japan)

    2005-08-15

    A glass sample of composition Bi{sub 4}Ti{sub 3}O{sub 12} was prepared by rapid quenching. The as-quenched sample was confirmed to be amorphous by synchrotron X-ray measurements. The crystallization process of the amorphous sample was also investigated by high-energy X-ray diffraction and by atomic pair distribution function analysis. The perovskite layer in the crystal Bi{sub 4}Ti{sub 3}O{sub 12} is transformed to a pyrochlore structure in the amorphous sample. The amorphous sample first crystallized to a metastable phase by acquiring long-range ordering of the pyrochlore structure at T {sub cryst1}, and then secondary crystallized into a reverted Bi{sub 4}Ti{sub 3}O{sub 12} structure at T {sub cryst2}.

  14. Surface and bulk crystallization of amorphous solid water films: Confirmation of “top-down” crystallization

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Chunqing; Smith, R. Scott; Kay, Bruce D.

    2016-10-01

    The crystallization kinetics of nanoscale amorphous solid water (ASW) films are investigated using temperature-programmed desorption (TPD) and reflection absorption infrared spectroscopy (RAIRS). TPD measurements are used to probe surface crystallization and RAIRS measurements are used to probe bulk crystallization. Isothermal TPD results show that surface crystallization is independent of the film thickness (from 100 to 1000 ML). Conversely, the RAIRS measurements show that the bulk crystallization time increases linearly with increasing film thickness. These results suggest that nucleation and crystallization begin at the ASW/vacuum interface and then the crystallization growth front propagates linearly into the bulk. This mechanism was confirmed by selective placement of an isotopic layer (5% D2O in H2O) at various positions in an ASW (H2O) film. In this case, the closer the isotopic layer was to the vacuum interface, the earlier the isotopic layer crystallized. These experiments provide direct evidence to confirm that ASW crystallization in vacuum proceeds by a “top-down” crystallization mechanism.

  15. Lithium niobate bulk crystallization promoted by CO{sub 2} laser radiation

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, N.M., E-mail: nmferreira@ua.pt [i3N - Aveiro, Physics Department, Aveiro University, Campus Universitario de Santiago, 3810-193 Aveiro (Portugal); Costa, F.M. [i3N - Aveiro, Physics Department, Aveiro University, Campus Universitario de Santiago, 3810-193 Aveiro (Portugal); Nogueira, R.N. [Instituto de Telecomunicacoes, 3810-193 Aveiro (Portugal); Graca, M.P.F. [i3N - Aveiro, Physics Department, Aveiro University, Campus Universitario de Santiago, 3810-193 Aveiro (Portugal)

    2012-09-15

    Highlights: Black-Right-Pointing-Pointer Crystallization of LiNbO{sub 3} nanocrystals in a SiO{sub 2} matrix by CO{sub 2} laser irradiation process. Black-Right-Pointing-Pointer Samples heat-treated at 650 Degree-Sign C (4 h) and laser treated (4 W/500 s) show similar morphology. Black-Right-Pointing-Pointer Glass-ceramics produced by laser process requires a very low processing time. - Abstract: The crystallization induced by laser radiation is a very promising technique to promote glass/ceramic transformation, being already used to produce crystalline patterns on glass surfaces. In this work, a SiO{sub 2}-Li{sub 2}O-Nb{sub 2}O{sub 5} glass, prepared by the sol-gel route, was submitted to CO{sub 2} laser radiation and conventional heat-treatments in order to induce the LiNbO{sub 3} crystallization. The structure and morphology of the samples prepared by both routes was analyzed as a function of exposure time, radiation power and heat-treatment temperatures by XRD, Raman spectroscopy and SEM. The results reveal a correlation between the crystallization degree of LiNbO{sub 3} particles and glass matrix with the heat treatment type and experimental parameters. An heat-treatment at 650 Degree-Sign C/4 h was necessary to induce crystallization in heat treatments samples while 4 W/500 s was enough for laser radiation ones, corresponding a reduction time processing of {approx}14 000 s.

  16. Detached phenomenon: Its effect on the crystal quality of Ga{sub (1−x)}In{sub x}Sb bulk crystal grown by the VDS technique

    Energy Technology Data Exchange (ETDEWEB)

    Gadkari, Dattatray, E-mail: db.gadkari@gmail.com [Department of Physics, Mithibai College, Mumbai 400056 (India)

    2013-05-15

    Vertical directional solidification (VDS) technique is used on the combined growth principals of the conventional methods since 1994, which leads to the detached growth. For evaluation of the detached growth, five bulk ingots of indium doped gallium–antimonide GaSb:In (In = 0.5, 0.25, 0.15) have been grown – without the seed, without contact to the ampoule wall, without coating and without external pressure. The gap is attributed to compensate the differential thermal dilatation that is grown with the reduced diameter than the diameter of the ampoule. VDS experiments have been proved that the sum of the contact angle and growth angle is large enough to allow detachment without any additional pressure difference under the melt to offset hydrostatic pressure. A meniscus forms at the bottom of the melt, the capillarity effect establishes due to which spontaneous gap could be created by the melt free surface, thus no thermal shear stress and thermo-mechanical stresses at the interface. Detached grown bulk GaSb:In crystals showed superior crystal quality with the highest physical properties and mobility than the crystals grown ever. The axial and radial composition profile of the grown GaSb:In ingots showed variation ≤10%. From the conical region, dislocation density decreases in the growth direction and reaches less than 10{sup 3} cm{sup −2}. - Highlights: ► Detachment: without seed, without ampoule contact, without coating, without external pressure. ► Detached ingot growth samples showed the highest physical properties and the carrier mobility. ► Initial to final transition: in detached growth, dislocations decreases and less than 10{sup 3} cm{sup −2}. ► Detached samples: Raman spectrum shows only TO phonon (110) direction of single orientation. ► Detached ingot: FTIR shows highest transmissions % but decreases on increase doping in samples.

  17. Growth of single crystals of BaFe12O19 by solid state crystal growth

    Science.gov (United States)

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

    2016-10-01

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

  18. Surface deterioration of ammonium acid phthalate crystals

    Energy Technology Data Exchange (ETDEWEB)

    Barrus, D.M.; Blake, R.L.; Burek, A.J.

    1976-01-01

    In working with various acid phthalate crystals for low energy X-ray spectroscopy, we have observed a relatively rapid surface degradation of ammonium acid phthalate in comparison with similar crystals was observed. It was found that two different samples degraded in a few days upon exposure to high vacuum (10/sup -6/ - 10/sup -7/ torr). The same crystals showed similar effects when exposed to room atmosphere for two to three weeks. One of these crystals deteriorated while kept constantly in a desiccator jar for about two years. The desiccator environment seems to be the most favorable. The observed difference in the surface of these crystals might be described as a change from a transparent, glasslike condition to a white, powderlike haze somewhat akin to frosted glass. A two week exposure to vacuum for a freshly cleaved crystal caused the integrated coefficient of reflection at 23.6 A to decrease by a factor of 2.5. The degraded surface areas tend to form definite rhombohedral patterns. Since the external symmetry of ammonium acid phthalate crystals is rhombohedral, this suggests that the degradation we observe takes place in the form of large etched figures. A possible mechanism may be sublimation, which would proceed more rapidly in vacuum than in air. It is concluded that ammonium acid phthalate should be kept in a desiccator environment as much as possible. Exposures to vacuum should be brief and critical diffraction measurements should be done using a freshly cleaved surface.

  19. Synthesis and structural characterization of bulk Sb2Te3 single crystal

    Science.gov (United States)

    Sultana, Rabia; Gahtori, Bhasker; Meena, R. S.; Awana, V. P. S.

    2018-05-01

    We report the growth and characterization of bulk Sb2Te3 single crystal synthesized by the self flux method via solid state reaction route from high temperature melt (850˚C) and slow cooling (2˚C/hour) of constituent elements. The single crystal X-ray diffraction pattern showed the 00l alignment and the high crystalline nature of the resultant sample. The rietveld fitted room temperature powder XRD revealed the phase purity and rhombohedral structure of the synthesized crystal. The formation and analysis of unit cell structure further verified the rhombohedral structure composed of three quintuple layers stacked one over the other. The SEM image showed the layered directional growth of the synthesized crystal carried out using the ZEISS-EVOMA-10 scanning electron microscope The electrical resistivity measurement was carried out using the conventional four-probe method on a quantum design Physical Property Measurement System (PPMS). The temperature dependent electrical resistivity plot for studied Sb2Te3 single crystal depicts metallic behaviour in the absence of any applied magnetic field. The synthesis as well as the structural characterization of as grown Sb2Te3 single crystal is reported and discussed in the present letter.

  20. Electron microscopy study of Ni induced crystallization in amorphous Si thin films

    International Nuclear Information System (INIS)

    Radnóczi, G. Z.; Battistig, G.; Pécz, B.; Dodony, E.; Vouroutzis, N.; Stoemenos, J.; Frangis, N.; Kovács, A.

    2015-01-01

    The crystallization of amorphous silicon is studied by transmission electron microscopy. The effect of Ni on the crystallization is studied in a wide temperature range heating thinned samples in-situ inside the microscope. Two cases of limited Ni source and unlimited Ni source are studied and compared. NiSi 2 phase started to form at a temperature as low as 250°C in the limited Ni source case. In-situ observation gives a clear view on the crystallization of silicon through small NiSi 2 grain formation. The same phase is observed at the crystallization front in the unlimited Ni source case, where a second region is also observed with large grains of Ni 3 Si 2 . Low temperature experiments show, that long annealing of amorphous silicon at 410 °C already results in large crystallized Si regions due to the Ni induced crystallization

  1. Growth and characterization of LiInSe2 single crystals

    Science.gov (United States)

    Ma, Tianhui; Zhu, Chongqiang; Lei, Zuotao; Yang, Chunhui; Sun, Liang; Zhang, Hongchen

    2015-04-01

    Large and crack-free LiInSe2 single crystals were obtained by the vertical gradient freezing method with adding a temperature oscillation technology in a two-zone furnace. X-ray diffraction data showed that the pure LiInSe2 compound was synthesized. The grown crystals had different color depending on melt composition. The atomic ratios of elements of LiInSe2 crystals were obtained by an Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES), and the structural formula were calculated according to the relative contents of elements. The average absorption coefficients were estimated by using average reflection indices. The absorption coefficients of the thermal annealing samples are 0.6 cm-1 at 2-3 μm. The transparent range of our LiInSe2 crystals is from 0.6 μm to 13.5 μm.

  2. Crystallization in lead tungsten fluorophosphate glasses

    International Nuclear Information System (INIS)

    Nardi, R.P.R.D.; Braz, C.E.; Cassanjes, F.C.; Poirier, G.

    2014-01-01

    The glass forming ability was investigated in the ternary system NaPO 3 -WO 3 -PbF 2 with a constant NaPO 3 /WO 3 ratio of 3/2 and increasing amounts of PbF 2 . It has been found that glass samples can be obtained from PbF 2 contents from 0 mole% to 60 mole%. The most lead fluoride concentrated samples (50% and 60%) were chosen for a crystallization study in order to investigate the possibility of obtaining glass-ceramics containing crystalline lead fluoride. DSC measurements allowed to determine the characteristic temperatures such as Tg, Tx, Tp and Tf. These glass samples were heat-treated near the crystallization peaks observed by thermal analysis. X-ray diffraction results of these heat-treated glasses pointed out that the dominant phase which precipitates from the glass sample containing 50% of PbF 2 is the lead fluorophosphates phase Pb 5 F(PO 4 ) 3 whereas the sample containing 60% of PbF 2 exhibits a preferential crystallization of cubic lead fluoride β-PbF 2 . (author)

  3. Growth, optical, ICP and thermal studies of nonlinear optical single crystal: Sodium acid phthalate (NaAP)

    Science.gov (United States)

    Mahadevan, M.; Arivanandhan, M.; Elangovan, K.; Anandan, P.; Ramachandran, K.

    2017-07-01

    Good quality single crystals of sodium acid phthalate (NaAP) were grown by slow evaporation technique. Single crystal X-ray diffraction study of the grown crystal reveals that the crystal belongs to orthorhombic system with space group B2ab. Fourier transform infrared spectrum confirms the presence of the functional groups of the grown material. Inductively coupled plasma emission spectroscopy analysis is used to confirm the presence of Na element in the sample. Thermal analysis of the NaAP crystal shows that the crystal is stable up to 140°C. Optical transmittance of the grown crystal was recorded in the wavelength range from 200 and 800 nm using UV-Vis-NIR spectrophotometer. The second harmonic generation of NaAP was analysed using Kurtz powder technique.

  4. Influence of crystallization time on structural and morphological characteristics the precursor of zeolite MCM-22

    International Nuclear Information System (INIS)

    Barbosa, A.S.; Lima, L.A.; Sousa, B.V.; Santos, Everton R.F. dos; Rodrigues, M.G.F.

    2009-01-01

    The zeolite MCM-22 has been studied extensively as a promising catalyst because of the high thermal stability and high activity for acid catalysis and selectivity of molecular shape. The synthesis of MCM-22 is carried out by hydrothermal treatment and long times required for complete crystallization gradual growth of crystals of 10-14 days for the synthesis of static. This work aims to synthesize the precursor of zeolite MCM-22 using the method of hydrothermal synthesis with a reduction in crystallization time of 8 and 9 days. The precursor of zeolite MCM-22 was obtained using sources of silica, soda, deionized water and the director of structures hexametilenoimina (HMI). The samples were synthesized at 150° C for 8 to 9 days, with the following molar composition: 0.511 SiO 2 : 0.039 NaOH: 0.024 Al 2 O 3 : 23.06 H 2 O and subjected to characterizations by X-ray diffraction (XRD), scanning electron microscopy ( SEM) and energy dispersive (EDX). According to tests carried out showed that the hydrothermal treatment used to synthesize the precursor of zeolite MCM-22 was effective during times of crystallization of 8 and 9 days. The results for the micrographs showed that the samples consist of clusters and / or aggregates of small crystals. (author)

  5. Optical and X-ray absorption spectroscopy in lead doped lithium fluoride crystals

    Energy Technology Data Exchange (ETDEWEB)

    Somma, F; Aloe, P; D' Acapito, F; Montereali, R M; Polosan, S; Secu, M; Vincenti, M A, E-mail: somma@fis.uniroma3.it

    2010-11-15

    LiF:Pb doped crystals were successfully grown by Kyropoulos method, starting with drying powders. The presence of Pb{sup 2+} ions in the LiF crystals were evidenced by the absorption band at 278 nm and by 375 nm photoluminescence. The presence of some other Pb structures with oxygen compounds in the as made samples was evidenced, decreasing after some annealing procedures. The local environment and valence state of Pb in LiF were studied by X-ray Absorption Spectroscopy at the Pb L{sub III} and L{sub I} edges. XANES data reveal that Pb is present as Pb{sup 2+} whereas EXAFS data show that it is incorporated in the crystal and not forming PbF{sub 2} precipitates. Identical spectra are obtained for samples as prepared and after thermal annealing up to 650 deg. C demonstrating the stability of the incorporation site. Also the concentration of Pb in the crystal has no effect on the location site of the metal as the same spectrum is obtained for specimens with different dopant concentrations.

  6. Ultrasmall-angle X-ray scattering analysis of photonic crystal structure

    International Nuclear Information System (INIS)

    Abramova, V. V.; Sinitskii, A. S.; Grigor'eva, N. A.; Grigor'ev, S. V.; Belov, D. V.; Petukhov, A. V.; Mistonov, A. A.; Vasil'eva, A. V.; Tret'yakov, Yu. D.

    2009-01-01

    The results of an ultrasmall-angle X-ray scattering study of iron(III) oxide inverse opal thin films are presented. The photonic crystals examined are shown to have fcc structure with amount of stacking faults varying among the samples. The method used in this study makes it possible to easily distinguish between samples with predominantly twinned fcc structure and nearly perfect fcc stacking. The difference observed between samples fabricated under identical conditions is attributed to random layer stacking in the self-assembled colloidal crystals used as templates for fabricating the inverse opals. The present method provides a versatile tool for analyzing photonic crystal structure in studies of inverse opals made of various materials, colloidal crystals, and three-dimensional photonic crystals of other types.

  7. Crystal growth and characterization of new semiorganic nonlinear optical single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Kulshrestha, Shobha, E-mail: shobha011986@gmail.com; Shrivastava, A. K., E-mail: ashwaniaks@rediffmail.com [School of Studies in Physics, Jiwaji University Gwalior (M.P.) – 474 011 (India)

    2016-05-06

    An organic material of a L-histidine monohydrochloride single crystal was grown in a distilled water solution using the slow evaporation method at 40–45°C. The grown crystal was transparent and colourless, with a size of about 20 × 9 × 5 mm{sup 3}, obtained within a period of 21 days. The solubility of grown crystals have found out at various temperatures. The UV-visible transmittance studies show that the grown crystals have wide optical transparency in the entire visible region It is observed that the crystal has transparency window from 255nm to 700nm and its energy gap (Eg) found to be is 3.1eV. The grown crystal was subjected to powder X-ray diffraction analysis, confirming that the orthorhombic crystalline nature of the crystal. To identify the surface morphology, the as grown crystal was subjected to FE-SEM technique. The chemical composition of the grown crystal was estimated by Energy dispersive X-ray analysis. The optical behaviour of the grown crystal was analyzed by PL study.

  8. Concanavalin A-binding cholesterol crystallization inhibiting and promoting activity in bile from patients with Crohn's disease compared to patients with ulcerative colitis.

    Science.gov (United States)

    Keulemans, Y C; Mok, K S; Slors, J F; Brink, M A; Gouma, D J; Tytgat, G N; Groen, A K

    1999-10-01

    Crohn's disease is a risk factor for gallstone formation. In contrast, patients with ulcerative colitis have an incidence of gallstone formation comparable to the general population. The reason for this difference is not known. The aim of this study was to elucidate the factors controlling cholesterol crystallization in gallbladder bile of Crohn's disease and ulcerative colitis patients. Gallbladder bile was obtained by aspiration during bowel resections (26 Crohn's disease patients, 20 ulcerative colitis patients). Biliary lipid composition, crystal detection time and the effect of extraction of the concanavalin A-binding fraction on crystal formation were determined. Cholesterol crystals were present in seven of the 26 bile samples of Crohn's disease-patients and one of the 20 ulcerative colitis patients. Four of the bile samples of Crohn's disease patients were fast nucleating. None of the 20 ulcerative colitis patients had fast nucleating bile. Lipid composition, total lipid concentration and CSI were not significantly different between the two groups. In Crohn's disease patients extraction of concanavalin A-binding fraction decreased crystallization in 10 bile samples but accelerated crystallization in one bile sample. In eight bile samples from ulcerative colitis patients crystallization increased after concanavalin A-binding fraction extraction. Compared to ulcerative colitis patients, gallbladder bile of Crohn's disease patients showed increased cholesterol crystallization despite comparable lipid composition and cholesterol saturation index. This difference is caused by increased cholesterol crystallization-promoting activity. Bile from ulcerative colitis patients contains a Con A-binding factor which inhibits cholesterol crystallization.

  9. Radiation damage in BaF2 crystals

    International Nuclear Information System (INIS)

    Woody, C.L.; Kierstead, J.A.; Levy, P.W.; Stoll, S.

    1991-01-01

    The effects of radiation damage and recovery have been studied in BaF 2 crystals exposed to 60 Co radiation. The change in optical transmission and scintillation light output have been measured as a function of dose up to 4.7 x 10 6 rad. Although some crystals exhibit a small change in transmission, a greater change in scintillation light output is observed. Several 25 cm long crystals whichhave been irradiated show large changes in both transmission and light output. Recovery from radiation damage has been studied as a function of time and exposure to UV light. A long lived radiation induced phosphorescence has been observed in all irradiated samples which is distinct from the standard fast and slow scintillation emissions. The emission spectrum of the phosphorescence has been measured and shown a peakat ∼330 nm, near the region of the slow scintillation component. Results are given on the dependence of the decay time of the phosphorescence with dose

  10. Single crystal growth and nonlinear optical properties of Nd3+ doped STGS crystal for self-frequency-doubling application

    Science.gov (United States)

    Chen, Feifei; Wang, Lijuan; Wang, Xinle; Cheng, Xiufeng; Yu, Fapeng; Wang, Zhengping; Zhao, Xian

    2017-11-01

    The self-frequency-doubling crystal is an important kind of multi-functional crystal materials. In this work, Nd3+ doped Sr3TaGa3Si2O14 (Nd:STGS) single crystals were successfully grown by using Czochralski pulling method, in addition, the nonlinear and laser-frequency-doubling properties of Nd:STGS crystals were studied. The continuous-wave laser at 1064 nm was demonstrated along different physical axes, where the maximum output power was obtained to be 295 mW for the Z-cut samples, much higher than the Y-cut (242 mW) and X-cut (217 mW) samples. Based on the measured refractive indexes, the phase matching directions were discussed and determined for type I (42.5°, 30°) and type II (69.5°, 0°) crystal cuts. As expected, self-frequency-doubling green laser at 529 nm was achieved with output powers being around 16 mW and 12 mW for type I and type II configurations, respectively.

  11. Orientation of crystals in alanine dosimeter assessed by DRS, as seen in EPR spectra evaluation

    International Nuclear Information System (INIS)

    Grazyna Przybytniak; Zagorski, Z.P.

    1996-01-01

    The alanine dosimeter made for evaluation by diffuse light reflection spectrophotometry (ALA/DRS) does not show the effect of orientation of crystals. Supposed deviation from random orientation has been investigated by EPR spectroscopy. EPR investigation shows that in spite of the very fine size of L-alanine crystals, they are oriented in thin layers of the polyethylene matrix. Specially prepared films with deliberately well oriented crystals have confirmed this observation. Our ALA/DRS dosimeter can be evaluated by the EPR method for the concentration of free radicals, providing that the dominating crystal orientation in the dosimetric film is indicated on it as an arrow, and the sample is inserted into the magnetic cavity always in the same orientation as has been done during the calibration operation. (author). 6 refs., 2 figs

  12. Ion Density Analysis of Single-Stranded DNA in Liquid Crystal

    Science.gov (United States)

    Iwabata, Kazuki; Seki, Yasutaka; Toizumi, Ryota; Shimada, Yuki; Furue, Hirokazu; Sakaguchi, Kengo

    2013-09-01

    With the widespread use of liquid crystals (LCs) in liquid crystal displays, we have looked into the application of liquid crystals in biotechnology. The purpose of the study described here is to investigate the physical properties of DNA using LCs. Synthetic oligonucleotide molecules were dispersed in MLC6884, the sample injected into antiparallel cells, and the amount of mobile ions was measured. The LC cell doped with oligonucleotide molecules showed a sequence-dependent, specific correlation between oligonucleotide concentration and the amount of mobile ions in the LC cells. In the framework of the Stokes model and polyacrylamide gel electrophoresis (PAGE) analysis, we speculate that this result arises from the difference in ion mobility, which is caused by the shape of the oligonucleotide molecule in the LC.

  13. Synthesis of porous CuInS2 crystals

    International Nuclear Information System (INIS)

    Akaki, Yoji; Matsubara, Takanori; Ohno, Yuki; Momiki, Takanori; Ide, Kazuki

    2009-01-01

    CuInS 2 crystals were grown from starting materials CuCl 2 .2H 2 O, InCl 3 .4H 2 O and thiourea with ethylene glycol solution, that were placed into a flask, heated, and refluxed for 1 hour. The diffraction peaks only from CuInS 2 phase appear for all the samples. The morphology of CuInS 2 crystal was porous, and the porous crystals exist in two kinds. One kind was flower-like crystals which complexly lack the flakes, another one was sphere-like crystals existed with a number of the poles. The sizes of sphere-like porous crystals were approximately 1.0 μm. The specific surface area of the samples grown at 180 C and 600 rpm estimated approximately 30 m 2 /g. (copyright 2009 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  14. Slow positrons in single-crystal samples of Al and Al-AlxOy

    Science.gov (United States)

    Lynn, K. G.; Lutz, H.

    1980-11-01

    Well-characterized Al(111) and Al(100) samples were studied with monoenergetic positrons before and after exposure to oxygen. Both positronium-formation and positron-emission curves were obtained for various incident positron energies at sample temperatures ranging from 160-900 K. The orthopositronium decay signal provides a unique signature that the positron has emerged from the surface region of a clean metal. In the clean Al crystals part of the positronium formed near the surface is found to be associated with a temperature-activated process described as the thermally activated detrapping of a positron from a surface state. A simple positron diffusion model, including surface and vacancy trapping, is fitted to the positronium data and an estimate of the binding energy of the positron in this trap is made. The positron diffusion constant is found to have a negative temperature dependence before the onset of positron trapping at thermally generated monovacancies (>500 K), in reasonable agreement with theoretical predictions. The depth of the positron surface state is reduced or positronium is formed in the chemisorbed layer as oxygen is adsorbed on both Al sample surfaces, thus increasing the positronium fraction and decreasing the positron emission. At higher oxygen exposures [>500 L (1 L = 10-6 torr sec)] positron or positronium traps are generated in the overlayer and the positronium fraction is reduced. The amorphous-to-crystalline surface transition of AlxOy on Al is observed between 650 and 800 K by the change in the positronium fraction and is interpreted as the removal of trapping centers in the metal-oxide overlayer. At the higher temperatures and incident energies vacancy trapping is observed by the decrease in the positron diffusion length in both the clean and the underlying Al of the oxygen-exposed samples. Similar vacancy formation enthalpies for Al are extracted in both the clean and oxygen-covered samples by a simple model and are in good

  15. Structural and electrical properties of organic stilbazolium single crystal of DSCHS

    Science.gov (United States)

    Sundaram, S. John; Raj, A. Antony; Ramaclus, Jerald V.; Sagayaraj, P.

    2016-05-01

    Organic nonlinear optical crystal 4-N, N-Dimethyl Amino-4'N'-Methyl-Stilbazolium 3-Carboxy-4-Hydroxy benzenesulfonate (DSCHS) has been successfully grown from aqueous methanol solution by adopting slow solvent evaporation technique. Chemical composition of the sample was confirmed by CHN analysis. Powder X-ray diffraction analysis was carried out and it shows that DSCHS crystal belongs to triclinic structure with Pl space group. It is found that this material exhibits positive photoconductivity. Dielectric studies were also carried out for different temperature by varying the frequency.

  16. Conductive properties of switchable photoluminescence thermosetting systems based on liquid crystals.

    Science.gov (United States)

    Tercjak, Agnieszka; Gutierrez, Junkal; Ocando, Connie; Mondragon, Iñaki

    2010-03-16

    Conductive properties of different thermosetting materials modified with nematic 4'-(hexyl)-4-biphenyl-carbonitrile (HBC) liquid crystal and rutile TiO(2) nanoparticles were successfully studied by means of tunneling atomic force miscroscopy (TUNA). Taking into account the liquid crystal state of the HBC at room temperature, depending on both the HBC content and the presence of TiO(2) nanoparticles, designed materials showed different TUNA currents passed through the sample. The addition of TiO(2) nanoparticles into the systems multiply the detected current if compared to the thermosetting systems without TiO(2) nanoparticles and simultaneously stabilized the current passed through the sample, making the process reversible since the absolute current values were almost the same applying both negative and positive voltage. Moreover, thermosetting systems modified with liquid crystals with and without TiO(2) nanoparticles are photoluminescence switchable materials as a function of temperature gradient during repeatable heating/cooling cycle. Conductive properties of switchable photoluminescence thermosetting systems based on liquid crystals can allow them to find potential application in the field of photoresponsive devices, with a high contrast ratio between transparent and opaque states.

  17. Structural, spectroscopic and Thermal Studies of Potassium Di-hydrogen Citrate Crystal

    Directory of Open Access Journals (Sweden)

    N.D. Pandya

    2017-04-01

    Full Text Available Potassium dihydrogen citrate (KDC finds wide applications in food products. Pure potassium dihydrogen citrate crystal was grown by slow solvent evaporation technique at room temperature. Grown crystal exhibited needle like morphology. The powder XRD shows triclinic structure symmetry with lattice parameters a=11.820 Å, b=14.970 Å, c=9.442 Å with angles α = 91.60°, β = 93.35°, γ = 110°. The presence of various functional groups of grown crystal was confirmed by using FT-IR spectroscopy. The thermogram indicates the thermal stability of the sample up to 100oC and then decomposes slowly into oxide stage through two stages. The results are discussed here.

  18. Microphase Separation Controlled beta-Sheet Crystallization Kinetics in Fibrous Proteins

    International Nuclear Information System (INIS)

    Hu, X.; Lu, Q.; Kaplan, D.; Cebe, P.

    2009-01-01

    Silk is a naturally occurring fibrous protein with a multiblock chain architecture. As such, it has many similarities with synthetic block copolymers, including the possibility for e-sheet crystallization restricted within the crystallizable blocks. The mechanism of isothermal crystallization kinetics of e-sheet crystals in silk multiblock fibrous proteins is reported in this study. Kinetics theories, such as Avrami analysis which was established for studies of synthetic polymer crystal growth, are for the first time extended to investigate protein self-assembly in e-sheet rich Bombyx mori silk fibroin samples, using time-resolved Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC) and synchrotron real-time wide-angle X-ray scattering (WAXS). The Avrami exponent, n, was close to 2 for all methods and crystallization temperatures, indicating formation of e-sheet crystals in silk proteins is different from the 3-D spherulitic crystal growth found in synthetic polymers. Observations by scanning electron microscopy support the view that the protein structures vary during the different stages of crystal growth, and show a microphase separation pattern after chymotrypsin enzyme biodegradation. We present a model to explain the crystallization of the multiblock silk fibroin protein, by analogy to block copolymers: crystallization of e-sheets occurs under conditions of geometrical restriction caused by phase separation of the crystallizable and uncrystallizable blocks. This crystallization model could be widely applicable in other proteins with multiblock (i.e., crystallizable and noncrystallizable) domains.

  19. Annealing effect of H+ -implanted single crystal silicon on strain and crystal structure

    International Nuclear Information System (INIS)

    Duo Xinzhong; Liu Weili; Zhang Miao; Gao Jianxia; Fu Xiaorong; Lin Chenglu

    2000-01-01

    The work focuses on the rocking curves of H + -implanted single silicon crystal detected by Four-Crystal X-ray diffractometer. The samples were annealed under different temperatures. Lattice defect in H + -implanted silicon crystals was detected by Rutherford Backscattering Spectrometry. It appeared that H-related complex did not crush until annealing temperature reached about 400 degree C. At that temperature H 2 was formed, deflated in silicon lattice and strained the lattice. But defects did not come into being in large quantity. The lattice was undamaged. When annealing temperature reached 500 degree C, strain induced by H 2 deflation crashed the silicon lattice. A large number of defects were formed. At the same time bubbles in the crystal and blister/flaking on the surface could be observed

  20. Probabilistic approach to lysozyme crystal nucleation kinetics.

    Science.gov (United States)

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

    2015-09-01

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

  1. Spatial solitons in nonlinear photonic crystals

    DEFF Research Database (Denmark)

    Corney, Joel Frederick; Bang, Ole

    2000-01-01

    We study solitons in one-dimensional quadratic nonlinear photonic crystals with periodic linear and nonlinear susceptibilities. We show that such crystals support stable bright and dark solitons, even when the effective quadratic nonlinearity is zero.......We study solitons in one-dimensional quadratic nonlinear photonic crystals with periodic linear and nonlinear susceptibilities. We show that such crystals support stable bright and dark solitons, even when the effective quadratic nonlinearity is zero....

  2. Enhancing Entropy and Enthalpy Fluctuations to Drive Crystallization in Atomistic Simulations

    Science.gov (United States)

    Piaggi, Pablo M.; Valsson, Omar; Parrinello, Michele

    2017-07-01

    Crystallization is a process of great practical relevance in which rare but crucial fluctuations lead to the formation of a solid phase starting from the liquid. As in all first order first transitions, there is an interplay between enthalpy and entropy. Based on this idea, in order to drive crystallization in molecular simulations, we introduce two collective variables, one enthalpic and the other entropic. Defined in this way, these collective variables do not prejudge the structure into which the system is going to crystallize. We show the usefulness of this approach by studying the cases of sodium and aluminum that crystallize in the bcc and fcc crystalline structures, respectively. Using these two generic collective variables, we perform variationally enhanced sampling and well tempered metadynamics simulations and find that the systems transform spontaneously and reversibly between the liquid and the solid phases.

  3. Primary crystallization in Al-rich metallic glasses at unusually low temperatures

    International Nuclear Information System (INIS)

    Bokeloh, J.; Boucharat, N.; Roesner, H.; Wilde, G.

    2010-01-01

    The initial stage of the primary crystallization reaction and the glass transition of the marginal metallic glass Al 89 Y 6 Fe 5 were investigated by conventional differential scanning calorimetry (DSC) and modulated differential scanning calorimetry (MDSC), microcalorimetry, X-ray diffraction (XRD) and transmission electron microscopy. A sharp onset of the primary crystallization was found by microcalorimetry and XRD studies at temperatures which were 120 deg. C below the primary crystallization peak observed in conventional DSC. A systematic MDSC study of annealed samples revealed a wide spectrum of glass transition onsets, which show a strong dependence on the annealing conditions. In addition, the glass transition onsets can be linked to the initial stage of the primary crystallization. The spectrum of glass transition onsets observed is discussed with respect to the occurrence of phase separation preceding the nucleation and growth of dendritic aluminium nanocrystals.

  4. Optical Studies on Sol-Gel Derived Lead Chloride Crystals

    OpenAIRE

    Rejeena, I; Lillibai, B; Nithyaja, B; Nampoori, P.N V; Radhakrishnan, P

    2013-01-01

    Optical characterization of lead chloride crystals prepared by sol-gel method is reported. The relevant sol-gel technique is used for the preparation of PbCl2 samples with five different types. In this paper, we report the absorption and fluorescence behaviour of pure, UV& IR irradiated and electric & magnetic field applied lead chloride crystal samples in solution phase at two different concentrations. Optical bandgap and emission studies of these crystals are also done.

  5. 3D imaging using X-Ray tomography and SEM combined FIB to study non isothermal creep damage of (111) oriented samples of γ / γ ′ nickel base single crystal superalloy MC2

    KAUST Repository

    Jouiad, Mustapha

    2012-01-01

    An unprecedented investigation consisting of the association of X-Ray tomography and Scanning Electron Microscopy combined with Focus Ion Beam (SEM-FIB) is conducted to perform a 3D reconstruction imaging. These techniques are applied to study the non-isothermal creep behavior of close (111) oriented samples of MC2 nickel base superalloys single crystal. The issue here is to develop a strategy to come out with the 3D rafting of γ\\' particles and its interaction whether with dislocation structures or/and with the preexisting voids. This characterization is uncommonly performed away from the conventional studied orientation [001] in order to feed the viscoplastic modeling leading to its improvement by taking into account the crystal anisotropy. The creep tests were performed at two different conditions: classical isothermal tests at 1050°C under 140 MPa and a non isothermal creep test consisting of one overheating at 1200°C and 30 seconds dwell time during the isothermal creep life. The X-Ray tomography shows a great deformation heterogeneity that is pronounced for the non-isothermal tested samples. This deformation localization seems to be linked to the preexisting voids. Nevertheless, for both tested samples, the voids coalescence is the precursor of the observed damage leading to failure. SEM-FIB investigation by means of slice and view technique gives 3D views of the rafted γ\\' particles and shows that γ corridors evolution seems to be the main creep rate controlling parameter. © 2012 Trans Tech Publications, Switzerland.

  6. Comparative Analysis of Clinical Samples Showing Weak Serum Reaction on AutoVue System Causing ABO Blood Typing Discrepancies.

    Science.gov (United States)

    Jo, Su Yeon; Lee, Ju Mi; Kim, Hye Lim; Sin, Kyeong Hwa; Lee, Hyeon Ji; Chang, Chulhun Ludgerus; Kim, Hyung Hoi

    2017-03-01

    ABO blood typing in pre-transfusion testing is a major component of the high workload in blood banks that therefore requires automation. We often experienced discrepant results from an automated system, especially weak serum reactions. We evaluated the discrepant results by the reference manual method to confirm ABO blood typing. In total, 13,113 blood samples were tested with the AutoVue system; all samples were run in parallel with the reference manual method according to the laboratory protocol. The AutoVue system confirmed ABO blood typing of 12,816 samples (97.7%), and these results were concordant with those of the manual method. The remaining 297 samples (2.3%) showed discrepant results in the AutoVue system and were confirmed by the manual method. The discrepant results involved weak serum reactions (serum reactions, samples from patients who had received stem cell transplants, ABO subgroups, and specific system error messages. Among the 98 samples showing ≤1+ reaction grade in the AutoVue system, 70 samples (71.4%) showed a normal serum reaction (≥2+ reaction grade) with the manual method, and 28 samples (28.6%) showed weak serum reaction in both methods. ABO blood tying of 97.7% samples could be confirmed by the AutoVue system and a small proportion (2.3%) needed to be re-evaluated by the manual method. Samples with a 2+ reaction grade in serum typing do not need to be evaluated manually, while those with ≤1+ reaction grade do.

  7. Crystallization in lead tungsten fluorophosphate glasses

    Energy Technology Data Exchange (ETDEWEB)

    Nardi, R.P.R.D.; Braz, C.E.; Cassanjes, F.C.; Poirier, G., E-mail: gael.poirier@unifal-mg.edu.br [Universidade Federal de Alfenas (UNIFAL), Pocos de Caldas, MG (Brazil). Instituto de Ciencia e Tecnologia

    2014-07-01

    The glass forming ability was investigated in the ternary system NaPO{sub 3}-WO{sub 3}-PbF{sub 2} with a constant NaPO{sub 3}/WO{sub 3} ratio of 3/2 and increasing amounts of PbF{sub 2}. It has been found that glass samples can be obtained from PbF{sub 2} contents from 0 mole% to 60 mole%. The most lead fluoride concentrated samples (50% and 60%) were chosen for a crystallization study in order to investigate the possibility of obtaining glass-ceramics containing crystalline lead fluoride. DSC measurements allowed to determine the characteristic temperatures such as Tg, Tx, Tp and Tf. These glass samples were heat-treated near the crystallization peaks observed by thermal analysis. X-ray diffraction results of these heat-treated glasses pointed out that the dominant phase which precipitates from the glass sample containing 50% of PbF{sub 2} is the lead fluorophosphates phase Pb{sub 5}F(PO{sub 4}){sub 3} whereas the sample containing 60% of PbF{sub 2} exhibits a preferential crystallization of cubic lead fluoride β-PbF{sub 2}. (author)

  8. Crystal structure prediction of flexible molecules using parallel genetic algorithms with a standard force field.

    Science.gov (United States)

    Kim, Seonah; Orendt, Anita M; Ferraro, Marta B; Facelli, Julio C

    2009-10-01

    This article describes the application of our distributed computing framework for crystal structure prediction (CSP) the modified genetic algorithms for crystal and cluster prediction (MGAC), to predict the crystal structure of flexible molecules using the general Amber force field (GAFF) and the CHARMM program. The MGAC distributed computing framework includes a series of tightly integrated computer programs for generating the molecule's force field, sampling crystal structures using a distributed parallel genetic algorithm and local energy minimization of the structures followed by the classifying, sorting, and archiving of the most relevant structures. Our results indicate that the method can consistently find the experimentally known crystal structures of flexible molecules, but the number of missing structures and poor ranking observed in some crystals show the need for further improvement of the potential. Copyright 2009 Wiley Periodicals, Inc.

  9. Neutron scattering experiments of the ionic crystal deformed plastically with uniaxial compression under high temperature

    Energy Technology Data Exchange (ETDEWEB)

    Tsuchiya, Yoshinori; Minakawa, Nobuaki; Aizawa, Kazuya; Ozawa, Kunio [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment

    1996-04-01

    As an aim of huge growth of alkali halide (AH) single crystal, a mosaic structure of small size AH single crystal deformed plastically with uniaxial compression under high temperature was evaluated due to its neutron irradiation experiment. Using TAS-2 installed at JRR-3M guide hole of Japan Atomic Energy Research Institute, locking curve at a representative face factor of the specimen was measured to observe the mosaic structure accompanied with expansion of the crystal due to compression. As a result, though the specimen before compression could be supposed to be divided to some parts already, the locking curve under 10 sec. of compression time showed already some fracture to divisions to suppose finer degradation of the crystal, and division of the locking curve at 600 sec. of compression time could be observed onto its 220 face. And, every compressed specimens showed some changes of crystallization method from standard sample. (G.K.)

  10. Maximizing Macromolecule Crystal Size for Neutron Diffraction Experiments

    Science.gov (United States)

    Judge, R. A.; Kephart, R.; Leardi, R.; Myles, D. A.; Snell, E. H.; vanderWoerd, M.; Curreri, Peter A. (Technical Monitor)

    2002-01-01

    A challenge in neutron diffraction experiments is growing large (greater than 1 cu mm) macromolecule crystals. In taking up this challenge we have used statistical experiment design techniques to quickly identify crystallization conditions under which the largest crystals grow. These techniques provide the maximum information for minimal experimental effort, allowing optimal screening of crystallization variables in a simple experimental matrix, using the minimum amount of sample. Analysis of the results quickly tells the investigator what conditions are the most important for the crystallization. These can then be used to maximize the crystallization results in terms of reducing crystal numbers and providing large crystals of suitable habit. We have used these techniques to grow large crystals of Glucose isomerase. Glucose isomerase is an industrial enzyme used extensively in the food industry for the conversion of glucose to fructose. The aim of this study is the elucidation of the enzymatic mechanism at the molecular level. The accurate determination of hydrogen positions, which is critical for this, is a requirement that neutron diffraction is uniquely suited for. Preliminary neutron diffraction experiments with these crystals conducted at the Institute Laue-Langevin (Grenoble, France) reveal diffraction to beyond 2.5 angstrom. Macromolecular crystal growth is a process involving many parameters, and statistical experimental design is naturally suited to this field. These techniques are sample independent and provide an experimental strategy to maximize crystal volume and habit for neutron diffraction studies.

  11. Progress on photonic crystals

    CERN Document Server

    Lecoq, P; Gundacker, S; Hillemanns, H; Jarron, P; Knapitsch, A; Leclercq, J L; Letartre, X; Meyer, T; Pauwels, K; Powolny, F; Seassal, C

    2010-01-01

    The renewal of interest for Time of Flight Positron Emission Tomography (TOF PET) has highlighted the need for increasing the light output of scintillating crystals and in particular for improving the light extraction from materials with a high index of refraction. One possible solution to overcome the problem of total internal reflection and light losses resulting from multiple bouncing within the crystal is to improve the light extraction efficiency at the crystal/photodetector interface by means of photonic crystals, i.e. media with a periodic modulation of the dielectric constant at the wavelength scale. After a short reminder of the underlying principles this contribution proposes to present the very encouraging results we have recently obtained on LYSO pixels and the perspectives on other crystals such as BGO, LuYAP and LuAG. These results confirm the impressive predictions from our previously published Monte Carlo simulations. A detailed description of the sample preparation procedure is given as well ...

  12. Antisolvent precipitation technique: A very promising approach to crystallize curcumin in presence of polyvinyl pyrrolidon for solubility and dissolution enhancement.

    Science.gov (United States)

    Sadeghi, Fatemeh; Ashofteh, Mohammad; Homayouni, Alireza; Abbaspour, Mohammadreza; Nokhodchi, Ali; Garekani, Hadi Afrasiabi

    2016-11-01

    Curcumin with a vast number of pharmacological activities is a poorly water soluble drug which its oral bioavailability is profoundly limited by its dissolution or solubility in GI tract. Curcumin could be a good anticancer drug if its solubility could be increased. Therefore, the aim of the present study was to increase the dissolution rate of curcumin by employing antisolvent crystallization technique and to investigate the effect of polyvinyl pyrrolidone K30 (PVP) as colloidal particles in crystallization medium on resultant particles. Curcumin was crystalized in the presence of different amounts of PVP by antisolvent crystallization method and their physical mixtures were prepared for comparison purposes. The samples were characterized by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), X-ray powder diffraction (XRPD) and Fourier transform infrared spectroscopy (FT-IR). The solubility and dissolution of the treated and untreated curcumin were also determined. Antisolvent crystallization of curcumin led to the formation of particles with no definite geometric shape. It was interesting to note that the DSC and XRPD studies indicated the formation of a new polymorph and less crystallinity for particles crystallized in the absence of PVP. However, the crystallized curcumin in the presence of PVP was completely amorphous. All crystalized curcumin samples showed much higher dissolution rate compared to untreated curcumin. The amount of curcumin dissolved within 10 for treated curcumin in the presence of PVP (1:1 curcumin:PVP) was 7 times higher than untreated curcumin and this enhancement in the dissolution for curcumin samples crystallized in the absence of PVP was around 5 times. Overall' the results of this study showed that antisolvent crystallization method in the absence or presence of small amounts of PVP is very efficient in increasing the dissolution rate of curcumin to achieve better efficiency for curcumin. Copyright © 2016

  13. Structural and electrical properties of organic stilbazolium single crystal of DSCHS

    International Nuclear Information System (INIS)

    Sundaram, S. John; Ramaclus, Jerald V.; Sagayaraj, P.; Raj, A. Antony

    2016-01-01

    Organic nonlinear optical crystal 4-N, N-Dimethyl Amino-4’N’-Methyl-Stilbazolium 3-Carboxy-4-Hydroxy benzenesulfonate (DSCHS) has been successfully grown from aqueous methanol solution by adopting slow solvent evaporation technique. Chemical composition of the sample was confirmed by CHN analysis. Powder X-ray diffraction analysis was carried out and it shows that DSCHS crystal belongs to triclinic structure with Pl space group. It is found that this material exhibits positive photoconductivity. Dielectric studies were also carried out for different temperature by varying the frequency.

  14. Shear effects on crystallization behaviors and structure transitions of isotactic poly-1-butene

    DEFF Research Database (Denmark)

    Li, Jingqing; Guan, Peipei; Zhang, Yao

    2014-01-01

    Different melt pre-shear conditions were applied to isotactic poly-1-butene (iP-1-B) and the effect on the crystallization behaviors and the crystalline structure transitions of iP-1-B were investigated. The polarized optical microscope observations during isothermal crystallization process...... revealed that the applied melt pre-shear within the experimental range could enhance the nucleation of crystal II and accelerate the diameter growth of the formed spherulites. If the applied melt pre-shear rate was large enough, Shish-Kebabs structure could be formed. After the isothermal crystallization...... was formed in the melt pre-sheared iP-1-B samples. Further investigations were applied with synchrotron radiation instruments. Wide angle X-ray scattering (WAXS) and small angle X-ray scattering (SAXS) after the crystal transition showed that the applied melt pre-shear could result in orientated fine...

  15. Crystallization Mechanism and Kinetics of BaO-Li2O-ZrO2-SiO2 Glasses

    Directory of Open Access Journals (Sweden)

    Cristian Berto da Silveira

    2002-03-01

    Full Text Available Differential thermal analysis and scanning electron microscopy were used to determine the influence of the addition of BaO on the crystallization mechanism of Li2O-ZrO2-SiO2 systems. As the concentration of BaO in the samples increased, a transition occurred in the predominant crystallization mechanism, which passed from superficial to volumetric. To determine the maximum nucleation rate, the crystallization kinetics of the sample containing 20 mole % BaO, which showed the most uniform crystallization, was studied by counting the nuclei with an image analyzer. The first nuclei appeared at the first endothermic inflection point (at the start of Tg, at 440 °C, while the maximum number of nuclei was counted at the midpoint of the glass transition region (446 °C. These results are similar to those observed for other materials that crystallize in volume, and confirm scanning electron microscopy data.

  16. Hopper Growth of Salt Crystals.

    Science.gov (United States)

    Desarnaud, Julie; Derluyn, Hannelore; Carmeliet, Jan; Bonn, Daniel; Shahidzadeh, Noushine

    2018-06-07

    The growth of hopper crystals is observed for many substances, but the mechanism of their formation remains ill understood. Here we investigate their growth by performing evaporation experiments on small volumes of salt solutions. We show that sodium chloride crystals that grow very fast from a highly supersaturated solution form a peculiar form of hopper crystal consisting of a series of connected miniature versions of the original cubic crystal. The transition between cubic and such hopper growth happens at a well-defined supersaturation where the growth rate of the cubic crystal reaches a maximum (∼6.5 ± 1.8 μm/s). Above this threshold, the growth rate varies as the third power of supersaturation, showing that a new mechanism, controlled by the maximum speed of surface integration of new molecules, induces the hopper growth of cubic crystals in cascade.

  17. Magnetic, transport, and optical properties of Ca0.85Eu0.15MnO3 single crystal

    International Nuclear Information System (INIS)

    Naumov, S.V.; Loshkareva, N.N.; Mostovshchikova, E.V.; Solin, N.I.; Korolev, A.V.; Arbuzova, T.I.; Telegin, S.V.; Patrakov, E.I.

    2013-01-01

    Magnetic, transport and optical properties of the Ca 0.85 Eu 0.15 MnO 3 single crystal are studied and discussed in comparison with the properties of polycrystalline sample. The magnetic data show existence the two magnetic phase transitions under cooling: the transition near 150 K occurs from the paramagnetic orthorhombic to C-type antiferromagnetic monoclinic phase with the charge/orbital ordering in some part of the crystal; and at 90 K the transition from the paramagnetic to G-type antiferromagnetic phase takes place in another part of the crystal with the orthorhombic structure. The magnetoresistance of the Ca 0.85 Eu 0.15 MnO 3 single crystal has features at temperatures of these phase transitions. Differences in the properties of single crystal and polycrystalline sample with the same content of Eu are associated with the ordering of oxygen vacancies that appear under the crystal growth. The reflection spectra in infrared range confirm the existence of the electron conductivity in a narrow band at room temperature.

  18. Environmental studies on X- and γ-irradiated LiCsSO4 crystals

    International Nuclear Information System (INIS)

    Kassem, M.E.

    2003-01-01

    Thermoluminescence (TL) characteristics of LiCsSO 4 crystal have been studied after exposure to different doses of X and γ radiations. The glow curves showed TL response of three peaks at 75 deg. C, 125 deg. C and 250 deg. C. The structure of the glow peaks due to X-rays is quite different from that due to γ-rays. UV exposure yields a regeneration of the TL peaks for the post-irradiated samples with X- or γ-radiation with some changes in the peak structure especially the third peak. For the post-X-ray irradiated crystals, the area under the third glow peak (PK III) increased linearly with the integrated time of UV exposure till about 30 min after which no changes were observed; while, for the post-γ-irradiated crystals, two linear regions were observed. The models of the TL response for the post-irradiated samples as a result of exposure to UV are discussed

  19. Primary and secondary fragmentation of crystal-bearing intermediate magma

    Science.gov (United States)

    Jones, Thomas J.; McNamara, Keri; Eychenne, Julia; Rust, Alison C.; Cashman, Katharine V.; Scheu, Bettina; Edwards, Robyn

    2016-11-01

    Crystal-rich intermediate magmas are subjected to both primary and secondary fragmentation processes, each of which may produce texturally distinct tephra. Of particular interest for volcanic hazards is the extent to which each process contributes ash to volcanic plumes. One way to address this question is by fragmenting pyroclasts under controlled conditions. We fragmented pumice samples from Soufriere Hills Volcano (SHV), Montserrat, by three methods: rapid decompression in a shock tube-like apparatus, impact by a falling piston, and milling in a ball mill. Grain size distributions of the products reveal that all three mechanisms produce fractal breakage patterns, and that the fractal dimension increases from a minimum of 2.1 for decompression fragmentation (primary fragmentation) to a maximum of 2.7 by repeated impact (secondary fragmentation). To assess the details of the fragmentation process, we quantified the shape, texture and components of constituent ash particles. Ash shape analysis shows that the axial ratio increases during milling and that particle convexity increases with repeated impacts. We also quantify the extent to which the matrix is separated from the crystals, which shows that secondary processes efficiently remove adhering matrix from crystals, particularly during milling (abrasion). Furthermore, measurements of crystal size distributions before (using x-ray computed tomography) and after (by componentry of individual grain size classes) decompression-driven fragmentation show not only that crystals influence particular size fractions across the total grain size distribution, but also that free crystals are smaller in the fragmented material than in the original pumice clast. Taken together, our results confirm previous work showing both the control of initial texture on the primary fragmentation process and the contributions of secondary processes to ash formation. Critically, however, our extension of previous analyses to characterisation

  20. Dynamical magnetic properties of the spin ice crystal Dy2Ti2O7

    International Nuclear Information System (INIS)

    Shi Jing; Tang, Z.; Zhu, B.P.; Huang, P.; Yin, D.; Li, C.Z.; Wang, Y.; Wen, H.

    2007-01-01

    The measurements of AC susceptibility between 2 and 40 K from zero field to 4 T both along the (0 0 1) and (1 1 1) axis in single-crystal Dy 2 Ti 2 O 7 show that the spin freezing along the (1 1 1) axis has stronger frequency dependence and magnetic field dependence, and the starting freezing frequency of the single crystal is higher than that of the polycrystalline sample

  1. The density and compositional analysis of titanium doped sapphire single crystal grown by the Czocharlski method

    Science.gov (United States)

    Kusuma, H. H.; Ibrahim, Z.; Othaman, Z.

    2018-03-01

    Titanium doped sapphire (Ti:Al2O3) crystal has attracted attention not only as beautiful gemstones, but also due to their applications as high power laser action. It is very important crystal for tunable solid state laser. Ti:Al2O3 crystals have been success grown using the Czocharlski method with automatic diameter control (ADC) system. The crystals were grown with different pull rates. The structure of the crystal was characterized with X-Ray Diffraction (XRD). The density of the crystal was measurement based on the Archimedes principle and the chemical composition of the crystal was confirmed by the Energy Dispersive X-ray (EDX) Spectroscopy. The XRD patterns of crystals are showed single main peak with a high intensity. Its shows that the samples are single crystal. The Ti:Al2O3 grown with different pull rate will affect the distribution of the concentration of dopant Ti3+ and densities on the sapphire crystals boules as well on the crystal growth process. The increment of the pull rate will increase the percentage distribution of Ti3+ and on the densities of the Ti:Al2O3 crystal boules. This may be attributed to the speed factor of the pull rate of the crystal that then caused changes in the heat flow in the furnace and then causes the homogeneities is changed of species distribution of atoms along crystal.

  2. Applications of diamond crystal ATR FTIR spectroscopy to the characterization of ambers.

    Science.gov (United States)

    Guiliano, Michel; Asia, Laurence; Onoratini, Gérard; Mille, Gilbert

    2007-08-01

    Diamond crystal ATR FTIR spectroscopy is a rapid technique with virtually no sample preparation which requires small sample amounts and showed potential in the study of ambers. FTIR spectra of ambers present discriminating patterns and can be used to distinguish amber from immature resins as copal, to determine local or Baltic origin of archaeological ambers and to detect most of the falsifications encountered in the amber commercialisation.

  3. CRYSTAL simulation code and modeling of coherent effects in a bent crystal at the LHC

    Energy Technology Data Exchange (ETDEWEB)

    Sytov, A.I., E-mail: alex_sytov@mail.ru [Research Institute for Nuclear Problems, Belarusian State University, Bobruiskaya str., 11, 220030 Minsk (Belarus); INFN Sezione di Ferrara, Dipartimento di Fisica e Scienze della Terra, Università di Ferrara, Via Saragat 1, 44100 Ferrara (Italy); Tikhomirov, V.V., E-mail: vvtikh@mail.ru [Research Institute for Nuclear Problems, Belarusian State University, Bobruiskaya str., 11, 220030 Minsk (Belarus)

    2015-07-15

    A CRYSTAL simulation code for particle tracking in crystals is introduced. Its essence consists in both adequate and fast sampling of proton trajectories in crystals which is crucial for both correct description of experiments and quantitative prediction of new effects. The H8 single-pass experiment at the CERN SPS as well as 7 TeV proton deflection by a bent crystal at the LHC are simulated. We predict the existence of dechanneling peaks corresponding to the planar channeling oscillations as well as describe the possibility of their observation at high energies, specifically at the LHC energy. An effect of excess over the amorphous level of ionization losses in the channeling mode was also found at 7 TeV.

  4. Sample positioning effects in x-ray spectrometry

    International Nuclear Information System (INIS)

    Carpenter, D.

    Instrument error due to variation in sample position in a crystal x-ray spectrometer can easily exceed the total instrumental error. Lack of reproducibility in sample position in the x-ray optics is the single largest source of system error. The factors that account for sample positioning error are described, and many of the details of flat crystal x-ray optics are discussed

  5. Structural, mechanical and light yield characterisation of heat treated LYSO:Ce single crystals for medical imaging applications

    Energy Technology Data Exchange (ETDEWEB)

    Mengucci, P., E-mail: p.mengucci@univpm.it [Università Politecnica delle Marche, Via Brecce Bianche, 60131 Ancona (Italy); André, G. [Laboratoire Léon Brillouin, CEA-CNRS, CE-Saclay, 91191 Gif sur Yvette cedex (France); Auffray, E. [Department PH-CMX CERN, Route de Meyrin, 1211 Geneva 23 (Switzerland); Barucca, G. [Università Politecnica delle Marche, Via Brecce Bianche, 60131 Ancona (Italy); Cecchi, C. [Dipartimento di Fisica e Geologia, Università di Perugia, Via A. Pascoli, 06123 Perugia (Italy); Chipaux, R. [CEA DSM/IRFU/SEDI, CE-Saclay, 91191 Gif sur Yvette cedex (France); Cousson, A. [Laboratoire Léon Brillouin, CEA-CNRS, CE-Saclay, 91191 Gif sur Yvette cedex (France); Davì, F. [Università Politecnica delle Marche, Via Brecce Bianche, 60131 Ancona (Italy); Di Vara, N. [Department PH-CMX CERN, Route de Meyrin, 1211 Geneva 23 (Switzerland); Rinaldi, D.; Santecchia, E. [Università Politecnica delle Marche, Via Brecce Bianche, 60131 Ancona (Italy)

    2015-06-11

    Five single crystals of cerium-doped lutetium yttrium oxyorthosilicate (LYSO:Ce) grown by the Czochralski method were submitted to structural characterisation by X-ray (XRD) and neutron (ND) diffraction, scanning (SEM) and transmission (TEM) electron microscopy and energy dispersive microanalysis (EDS). The Ultimate Tensile Strength (UTS), the Young Modulus (YM) and the Light Yield (LY) of the samples were also measured in order to correlate the mechanical and the optical behaviour of the crystals with the characteristics of their microstructure. Two of the samples analysed were also heat treated at 300 °C for 10 h to evidence possible variations induced by the temperature in the optical and mechanical response of the crystals. Results showed that the mean compositional variations evidenced by the structural analyses do not affect the mechanical and optical behaviour of the samples. On the contrary, the thermal treatment could induce the formation of coherent spherical particles (size 10 to 15 nm), not uniformly distributed inside the sample, that strongly reduce the UTS and YM values, but it does not affect the optical response of the crystal. This latter result was attributed to the low value of the heating temperature (300 °C) that is not sufficiently high to induce annealing of the oxygen vacancies traps that are responsible of the deterioration of the scintillation properties of the LYSO:Ce crystals. This study was carried out in the framework of the Crystal Clear Collaboration (CCC)

  6. A Compact Device for Colloidal Crystal Studies on Tiangong-1 Target Spacecraft

    Science.gov (United States)

    Li, Xiao-Long; Hu, Shu-Xin; Sun, Zhi-Bin; Zhai, Yong-Liang; Wu, Lan-Sheng; Huang, Zhen; Li, Wei-Ning; Yang, Han-Dong; Zhai, Guang-Jie; Li, Ming

    2014-07-01

    An experimental device with three crystallization cells, each with two working positions, was designed to study growth kinetics and structural transformation of colloidal crystals under microgravity condition. The device is capable of remote control of experimental procedures. It uses direct-space imaging with white light to monitor morphology of the crystals and reciprocal-space laser diffraction (Kossel lines) to reveal lattice structure. The device, intended for colloidal crystal growth kinetics and structural transformation on Tiangong-1 target spacecraft, had run on-orbit for more than one year till the end of the mission. Hundreds of images and diffraction patterns were collected via the on-ground data receiving station. The data showed that single crystalline samples were successfully grown on the orbit. Structural transformation was carefully studied under electric and thermal field. Using a backup device, control experiments were also performed on the ground under similar conditions except for the microgravity. Preliminary results indicated that the on-orbit crystals were more stable than the on-ground ones.

  7. Study on sensing property of one-dimensional ring mirror-defect photonic crystal

    Science.gov (United States)

    Chen, Ying; Luo, Pei; Cao, Huiying; Zhao, Zhiyong; Zhu, Qiguang

    2018-02-01

    Based on the photon localization and the photonic bandgap characteristics of photonic crystals (PCs), one-dimensional (1D) ring mirror-defect photonic crystal structure is proposed. Due to the introduction of mirror structure, a defect cavity is formed in the center of the photonic crystal, and then the resonant transmission peak can be obtained in the bandgap of transmission spectrum. The transfer matrix method is used to establish the relationship model between the resonant transmission peak and the structure parameters of the photonic crystals. Using the rectangular air gate photonic crystal structure, the dynamic monitoring of the detected gas sample parameters can be achieved from the shift of the resonant transmission peak. The simulation results show that the Q-value can attain to 1739.48 and the sensitivity can attain to 1642 nm ṡ RIU-1, which demonstrates the effectiveness of the sensing structure. The structure can provide certain theoretical reference for air pollution monitoring and gas component analysis.

  8. Unique Crystal Orientation of Poly(ethylene oxide) Thin Films by Crystallization Using a Thermal Gradient

    DEFF Research Database (Denmark)

    Gbabode, Gabin; Delvaux, Maxime; Schweicher, Guillaume

    2017-01-01

    Poly(ethylene oxide), (PEO), thin films of different thicknesses (220, 450, and 1500 nm) and molecular masses (4000, 8000, and 20000 g/mol) have been fabricated by spin-coating of methanol solutions onto glass substrates. All these samples have been recrystallized from the melt using a directional......, to significantly decrease the distribution of crystal orientation obtained after crystallization using the thermal gradient technique....

  9. In situ monitoring of thermal crystallization of ultrathin tris(8-hydroxyquinoline) aluminum films using surface-enhanced Raman scattering.

    Science.gov (United States)

    Muraki, Naoki

    2014-01-01

    Thermal crystallization of 3, 10, and 60 nm-thick tris(8-hydroxyquinoline)aluminum (Alq3) films is studied using surface-enhanced Raman scattering with a constant heating rate. An abrupt higher frequency shift of the quinoline-stretching mode is found to be an indication of a phase transition of Alq3 molecules from amorphous to crystalline. While the 60 nm-thick film shows the same crystallization temperature as a bulk sample, the thinner films were found to have a lower crystallization temperature and slower rate of crystallization. Non-isothermal kinetics analysis is performed to quantify kinetic properties such as the Avrami exponent constants and crystallization rates of ultrathin Alq3 films.

  10. Hypersonic phononic crystals.

    Science.gov (United States)

    Gorishnyy, T; Ullal, C K; Maldovan, M; Fytas, G; Thomas, E L

    2005-03-25

    In this Letter we propose the use of hypersonic phononic crystals to control the emission and propagation of high frequency phonons. We report the fabrication of high quality, single crystalline hypersonic crystals using interference lithography and show that direct measurement of their phononic band structure is possible with Brillouin light scattering. Numerical calculations are employed to explain the nature of the observed propagation modes. This work lays the foundation for experimental studies of hypersonic crystals and, more generally, phonon-dependent processes in nanostructures.

  11. The MORPHEUS II protein crystallization screen

    Energy Technology Data Exchange (ETDEWEB)

    Gorrec, Fabrice, E-mail: fgorrec@mrc-lmb.cam.ac.uk [MRC Laboratory of Molecular Biology, Francis Crick Avenue, Cambridge Biomedical Campus, Cambridge CB2 0QH (United Kingdom)

    2015-06-27

    MORPHEUS II is a 96-condition initial crystallization screen formulated de novo. The screen incorporates reagents selected from the Protein Data Bank to yield crystals that are not observed in traditional conditions. In addition, the formulation facilitates the optimization and cryoprotection of crystals. High-quality macromolecular crystals are a prerequisite for the process of protein structure determination by X-ray diffraction. Unfortunately, the relative yield of diffraction-quality crystals from crystallization experiments is often very low. In this context, innovative crystallization screen formulations are continuously being developed. In the past, MORPHEUS, a screen in which each condition integrates a mix of additives selected from the Protein Data Bank, a cryoprotectant and a buffer system, was developed. Here, MORPHEUS II, a follow-up to the original 96-condition initial screen, is described. Reagents were selected to yield crystals when none might be observed in traditional initial screens. Besides, the screen includes heavy atoms for experimental phasing and small polyols to ensure the cryoprotection of crystals. The suitability of the resulting novel conditions is shown by the crystallization of a broad variety of protein samples and their efficiency is compared with commercially available conditions.

  12. The MORPHEUS II protein crystallization screen

    International Nuclear Information System (INIS)

    Gorrec, Fabrice

    2015-01-01

    MORPHEUS II is a 96-condition initial crystallization screen formulated de novo. The screen incorporates reagents selected from the Protein Data Bank to yield crystals that are not observed in traditional conditions. In addition, the formulation facilitates the optimization and cryoprotection of crystals. High-quality macromolecular crystals are a prerequisite for the process of protein structure determination by X-ray diffraction. Unfortunately, the relative yield of diffraction-quality crystals from crystallization experiments is often very low. In this context, innovative crystallization screen formulations are continuously being developed. In the past, MORPHEUS, a screen in which each condition integrates a mix of additives selected from the Protein Data Bank, a cryoprotectant and a buffer system, was developed. Here, MORPHEUS II, a follow-up to the original 96-condition initial screen, is described. Reagents were selected to yield crystals when none might be observed in traditional initial screens. Besides, the screen includes heavy atoms for experimental phasing and small polyols to ensure the cryoprotection of crystals. The suitability of the resulting novel conditions is shown by the crystallization of a broad variety of protein samples and their efficiency is compared with commercially available conditions

  13. An arc detector for neutron crystal structure investigations

    Energy Technology Data Exchange (ETDEWEB)

    Habib, N [Reactor and Neutron Physics Dept., Nuclear Research Center. AEA, Cairo (Egypt)

    1997-12-31

    An arc detector for neutron structure investigations of powder crystals using time-of-flight technique is described. In order to enable the measurement of integral intensity from about 1/4 of the Debye-Scherrer ring and for simplicity reasons, the scattering angle 20-90 degree was chosen and a special arc collimator was built. The arc collimator-detector had a divergency of about 20 minutes of arc, and the distance between detector-sample was 64 cm. Four {sup 3} He detectors were fixed on the arc of the collimator. Both efficiency and space sensitivity of the detector were determined using a point neutron source. Results of measurements show that parameters of the arc detector are acceptable for high resolution crystal structure investigations. 6 figs.

  14. Double ferromagnetism in single-crystal Gd-Y-Lu alloys

    International Nuclear Information System (INIS)

    Ito, T.; Oka, M.; Legvold, S.; Beaudry, B.J.

    1984-01-01

    Magnetization, electrical resistivity, specific-heat and thermal-expansion measurements have been made on Gd-Y-Lu single crystals. Low isofield magnetization data for the a-axis sample of Gd 75 Y/sub 17.5/ Lu/sub 7.5/ exhibit two different Curie-Weiss regimes, which suggests double ferromagnetism. Electrical resistivity, specific-heat, and thermal-expansion data show two anomalies at the transition temperatures. The anomaly at 231.5 K shows a lambda-type second-order phase transition and the anomaly at 223 K shows a sharp spike first-order phase transition

  15. Power law olivine crystal size distributions in lithospheric mantle xenoliths

    Science.gov (United States)

    Armienti, P.; Tarquini, S.

    2002-12-01

    Olivine crystal size distributions (CSDs) have been measured in three suites of spinel- and garnet-bearing harzburgites and lherzolites found as xenoliths in alkaline basalts from Canary Islands, Africa; Victoria Land, Antarctica; and Pali Aike, South America. The xenoliths derive from lithospheric mantle, from depths ranging from 80 to 20 km. Their textures vary from coarse to porphyroclastic and mosaic-porphyroclastic up to cataclastic. Data have been collected by processing digital images acquired optically from standard petrographic thin sections. The acquisition method is based on a high-resolution colour scanner that allows image capturing of a whole thin section. Image processing was performed using the VISILOG 5.2 package, resolving crystals larger than about 150 μm and applying stereological corrections based on the Schwartz-Saltykov algorithm. Taking account of truncation effects due to resolution limits and thin section size, all samples show scale invariance of crystal size distributions over almost three orders of magnitude (0.2-25 mm). Power law relations show fractal dimensions varying between 2.4 and 3.8, a range of values observed for distributions of fragment sizes in a variety of other geological contexts. A fragmentation model can reproduce the fractal dimensions around 2.6, which correspond to well-equilibrated granoblastic textures. Fractal dimensions >3 are typical of porphyroclastic and cataclastic samples. Slight bends in some linear arrays suggest selective tectonic crushing of crystals with size larger than 1 mm. The scale invariance shown by lithospheric mantle xenoliths in a variety of tectonic settings forms distant geographic regions, which indicate that this is a common characteristic of the upper mantle and should be taken into account in rheological models and evaluation of metasomatic models.

  16. Metadynamics studies of crystal nucleation

    Science.gov (United States)

    Giberti, Federico; Salvalaglio, Matteo; Parrinello, Michele

    2015-01-01

    Crystallization processes are characterized by activated events and long timescales. These characteristics prevent standard molecular dynamics techniques from being efficiently used for the direct investigation of processes such as nucleation. This short review provides an overview on the use of metadynamics, a state-of-the-art enhanced sampling technique, for the simulation of phase transitions involving the production of a crystalline solid. In particular the principles of metadynamics are outlined, several order parameters are described that have been or could be used in conjunction with metadynamics to sample nucleation events and then an overview is given of recent metadynamics results in the field of crystal nucleation. PMID:25866662

  17. Metadynamics studies of crystal nucleation

    Directory of Open Access Journals (Sweden)

    Federico Giberti

    2015-03-01

    Full Text Available Crystallization processes are characterized by activated events and long timescales. These characteristics prevent standard molecular dynamics techniques from being efficiently used for the direct investigation of processes such as nucleation. This short review provides an overview on the use of metadynamics, a state-of-the-art enhanced sampling technique, for the simulation of phase transitions involving the production of a crystalline solid. In particular the principles of metadynamics are outlined, several order parameters are described that have been or could be used in conjunction with metadynamics to sample nucleation events and then an overview is given of recent metadynamics results in the field of crystal nucleation.

  18. Synthesis of porous CuInS{sub 2} crystals

    Energy Technology Data Exchange (ETDEWEB)

    Akaki, Yoji; Matsubara, Takanori; Ohno, Yuki; Momiki, Takanori; Ide, Kazuki [Department of Electrical and Computer Engineering, Miyakonojo National College of Technology, 473-1 Yoshio, Miyakonojo, Miyazaki (Japan)

    2009-05-15

    CuInS{sub 2} crystals were grown from starting materials CuCl{sub 2}.2H{sub 2}O, InCl{sub 3}.4H{sub 2}O and thiourea with ethylene glycol solution, that were placed into a flask, heated, and refluxed for 1 hour. The diffraction peaks only from CuInS{sub 2} phase appear for all the samples. The morphology of CuInS{sub 2} crystal was porous, and the porous crystals exist in two kinds. One kind was flower-like crystals which complexly lack the flakes, another one was sphere-like crystals existed with a number of the poles. The sizes of sphere-like porous crystals were approximately 1.0 {mu}m. The specific surface area of the samples grown at 180 C and 600 rpm estimated approximately 30 m{sup 2}/g. (copyright 2009 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  19. Environmental studies on X- and {gamma}-irradiated LiCsSO{sub 4} crystals

    Energy Technology Data Exchange (ETDEWEB)

    Kassem, M.E

    2003-09-01

    Thermoluminescence (TL) characteristics of LiCsSO{sub 4} crystal have been studied after exposure to different doses of X and {gamma} radiations. The glow curves showed TL response of three peaks at 75 deg. C, 125 deg. C and 250 deg. C. The structure of the glow peaks due to X-rays is quite different from that due to {gamma}-rays. UV exposure yields a regeneration of the TL peaks for the post-irradiated samples with X- or {gamma}-radiation with some changes in the peak structure especially the third peak. For the post-X-ray irradiated crystals, the area under the third glow peak (PK III) increased linearly with the integrated time of UV exposure till about 30 min after which no changes were observed; while, for the post-{gamma}-irradiated crystals, two linear regions were observed. The models of the TL response for the post-irradiated samples as a result of exposure to UV are discussed.

  20. Shear and Rapeseed Oil Addition Affect the Crystal Polymorphic Behavior of Milk Fat

    DEFF Research Database (Denmark)

    Kaufmann, Niels; Kirkensgaard, Jacob Judas Kain; Andersen, Ulf

    2013-01-01

    The effect of shear on the crystallization kinetics of anhydrous milk fat (AMF) and blends with 20 and 30 % w/w added rapeseed oil (RO) was studied. Pulse 1H NMR was used to follow the a to b0 polymorphic transition. The NMR method was confirmed and supported by SAXS/WAXS experiments. Samples were...... faster in the presence of RO allowing more room for the conformational changes to occur. Final SFC decreased with increasing RO content. Shear applied in 20 and 30 % blends caused the destruction of b0-related 3L structure leaving only 2L packing. In AMF and statically crystallized samples, both 3L and 2......L packing existed. Shear did not affect the amount of b crystals formed. The study shows that both shear and RO affect the polymorphic behavior of milk fat, and that 1H NMR is able to detect polymorphic transition in blends with up to 30 % w/w RO....

  1. Crystallization induced of amorphous silicon by nickel

    International Nuclear Information System (INIS)

    Schmidt, J.A; Rinaldi, P; Budini, N; Arce, R; Buitrago, R.H

    2008-01-01

    Polycrystalline silicon (pc-Si) deposited on glass substrates is a very promising material for the production of different electronic devices, like thin film transistors, active matrices or solar cells. The crystallization of the amorphous silicon to obtain pc-Si can be achieved with different processes, among which nickel-induced crystallization is because it requires low concentrations of the metal and low annealing temperatures. Nucleation and growth of crystalline silicon are measured by the formation of silicide NiSi 2 , which has a lattice constant very similar to that of Si, and acts as a seed upon which crystalline grains can develop. The size of the pc-Si final grain depends on many factors, such as the initial concentration of Ni, the annealing time and temperature, and the presence of other atoms in the Si structure. This work presents a study on the influence of these parameters on the silicon crystallization process induced by Ni. We deposited a series of hydrogenated amorphous silicon samples (a-Si:H) on glass substrates, using the plasma-enhanced chemical vapor deposition method (PE-CVD) with silane gas (SiH 4 ). The deposition temperature was 200 o C, and we prepared intrinsic samples (i), lightly doped with boron (p), heavily doped with boron (p + ) and heavily doped with phosphorous (n + ). Each sample was divided into eight portions, depositing different concentrations of Ni into each one using the cathodic sputtering method. The concentration of Ni was determined by atomic adsorption spectroscopy, and included from 1.5 1 0 15 to 1.5 1 0 16 at/cm 2 . Later the samples were submitted to different thermal treatments in a circulating nitrogen atmosphere. In order to avoid violent dehydrogenation of the a-Si:H that damages the samples, the annealing was carried out gradually. In a first stage the samples were heated at a velocity of 0.5 o C /min up to 400 o C, holding them for 24 hrs at this temperature in order to reach hydrogen effusion. Heating

  2. Crystal growth, spectral properties, and laser demonstration of laser crystal Nd:LYSO

    Science.gov (United States)

    Li, D. Z.; Xu, X. D.; Zhou, D. H.; Zhuang, S. D.; Wang, Z. P.; Xia, C. T.; Wu, F.; Xu, J.

    2010-11-01

    A Nd:LYSO crystal has been grown by the Czochralski technique. The cell parameters were analyzed with X-ray diffraction (XRD). The Judd-Ofelt intense parameters Ω2,4,6 were obtained to be 2.65, 5.75, and 7.37×10-20 cm2, respectively. The absorption and emission cross sections and the branching ratios were calculated. The large absorption cross section (6.14×10-20 cm2) and broad absorption band (5 nm) around 811 nm indicate that this crystal can be pumped efficiently by laser diodes. The broad emission band from the 4F3/2 multiplet shows that the crystal is a promising medium for ultrashort pulse lasers. Pumped by a laser diode, the maximum 814 mW continuous-wave laser output has been obtained with a slope efficiency of 28.9%. All the results show that this crystal is a promising laser material.

  3. Crystal growth, spectral properties, and laser demonstration of laser crystal Nd:LYSO

    International Nuclear Information System (INIS)

    Li, D Z; Xu, X D; Zhou, D H; Xia, C T; Wu, F; Zhuang, S D; Wang, Z P; Xu, J

    2010-01-01

    A Nd:LYSO crystal has been grown by the Czochralski technique. The cell parameters were analyzed with X-ray diffraction (XRD). The Judd-Ofelt intense parameters Ω 2,4,6 were obtained to be 2.65, 5.75, and 7.37×10 -20 cm 2 , respectively. The absorption and emission cross sections and the branching ratios were calculated. The large absorption cross section (6.14×10 -20 cm 2 ) and broad absorption band (5 nm) around 811 nm indicate that this crystal can be pumped efficiently by laser diodes. The broad emission band from the 4 F 3/2 multiplet shows that the crystal is a promising medium for ultrashort pulse lasers. Pumped by a laser diode, the maximum 814 mW continuous-wave laser output has been obtained with a slope efficiency of 28.9%. All the results show that this crystal is a promising laser material

  4. Kinetic study of α-BZN crystallization obtained from chemical method

    Directory of Open Access Journals (Sweden)

    Ronaldo Rodrigues Pelá

    2008-09-01

    Full Text Available The crystallization kinetics of ceramics composed by Bi2O3-ZnO-Nb2O5 (BZN was studied using non-isothermal method. The BZN samples were prepared by the polymeric precursors method. Phase evolution was evaluated by X ray diffraction and the thermal events were evaluated by differential scanning calorimetry (DSC. The crystallization of BZN occurs from 500 to 700 °C, which corresponds to a secondary event in DSC curves. The principal exothermic event in these curves is related to the decomposition of organic material and was isolated from the crystallization peak by deconvolution into two Gaussian curves. Those related to crystallization processes were evaluated in terms of crystallized fraction. Kinetic parameters were determined from Ligero (E = 242 ± 7 kJ.mol-1 and Kissinger (E = 241 ± 24 kJ.mol-1 methodologies and they are very close. The activation energy Ea = (241 ± 24 kJ.mol-1 and (242 ± 7 kJ.mol-1 (by the Kissinger and Ligero methodology, respectively, frequency factor k0 =10(13.s-1 and exponent of Avrami n = (1.3 ± 0.1 were determined. The n value indicates that the crystallization is diffusion controlled, with decreasing nucleation rate. Scanning electronic microscopy showed the presence of nanoparticulated powder.

  5. Density of states controls Anderson localization in disordered photonic crystal waveguides

    DEFF Research Database (Denmark)

    Garcia-Fernández, David; Smolka, Stephan; Stobbe, Søren

    2010-01-01

    We prove Anderson localization in a disordered photonic crystal waveguide by measuring the ensemble-averaged extinction mean-free path, ℓe, which is controlled by the dispersion in the photon density of states (DOS) of the photonic crystal waveguide. Except for the very low DOS case, where out......-of-plane losses are non-negligible, ℓe can be approximated to be the localization length ξ. The extinction mean-free path shows a fivefold variation between the low- and the high-DOS regime, and it becomes shorter than the sample length thus giving rise to strongly confined modes. The dispersive behavior of ℓe...

  6. Phonon assisted electronic transition in telluric acid ammonium phosphate single crystals

    Science.gov (United States)

    El-Muraikhi, M.; Kassem, M. E.; Al-Houty, L.

    The effect of gamma-irradiation on the absorption optical spectra of telluric acid ammonium phosphate single crystals (TAAP) has been studied, in the wave length of 200-600 nm, for samples irradiated by various doses up to 10 Mrad. The results show that the electron phonon coupling constant increases with the irradiation dose.

  7. Crystal growth, spectral and laser properties of Nd:LuAG single crystal

    International Nuclear Information System (INIS)

    Xu, X D; Meng, J Q; Cheng, Y; Li, D Z; Cheng, S S; Wu, F; Zhao, Z W; Wang, X D; Xu, J

    2009-01-01

    Nd:LuAG (Nd:Lu 3 Al 5 O 12 ) crystal was grown by the Czochralski method. X-ray powder diffraction experiments show that the Nd:LuAG crystal crystallizes in the cubic with space group Ia3d and has the cell parameter: a = 1.1907 nm, V = 1.6882 nm 3 . The absorption and fluorescence spectra of Nd:LuAG crystal at room temperature were investigated. With a fiber-coupled diode laser as pump source, the continuous-wave (CW) laser action of Nd:LuAG crystal was demonstrated. The maximum output power at 1064 nm was obtained to be 3.8 W under the incident pump power of 17.3 W, with the optical conversion efficiency 22.0% and the slope efficiency 25.7%

  8. Crystal growth, spectral and laser properties of Nd:LuAG single crystal

    Science.gov (United States)

    Xu, X. D.; Wang, X. D.; Meng, J. Q.; Cheng, Y.; Li, D. Z.; Cheng, S. S.; Wu, F.; Zhao, Z. W.; Xu, J.

    2009-09-01

    Nd:LuAG (Nd:Lu3Al5O12) crystal was grown by the Czochralski method. X-ray powder diffraction experiments show that the Nd:LuAG crystal crystallizes in the cubic with space group Ia3d and has the cell parameter: a = 1.1907 nm, V = 1.6882 nm3. The absorption and fluorescence spectra of Nd:LuAG crystal at room temperature were investigated. With a fiber-coupled diode laser as pump source, the continuous-wave (CW) laser action of Nd:LuAG crystal was demonstrated. The maximum output power at 1064 nm was obtained to be 3.8 W under the incident pump power of 17.3 W, with the optical conversion efficiency 22.0% and the slope efficiency 25.7%.

  9. Radiation-electromagnetic effect in germanium single crystals

    International Nuclear Information System (INIS)

    Kikoin, I.K.; Kikoin, L.I.; Lazarev, S.D.

    1980-01-01

    An experimental study was made of the radiation-electromagnetic effect in germanium single crystals when excess carriers were generated by bombardment with α particles, protons, or x rays in magnetic fields up to 8 kOe. The source of α particles and protons was a cyclotron and x rays were provided by a tube with a copper anode. The radiation-electromagnetic emf increased linearly on increase in the magnetic field and was directly proportional to the flux of charged particles at low values of the flux, reaching saturation at high values of the flux (approx.5 x 10 11 particles .cm -2 .sec -1 ). In the energy range 4--40 MeV the emf was practically independent of the α-particle energy. The sign of the emf was reversed when samples with a ground front surface were irradiated. Measurements of the photoelectromagnetic and Hall effects in the α-particle-irradiated samples showed that a p-n junction was produced by these particles and its presence should be allowed for in investigations of the radiation-electromagnetic effect. The measured even radiation-electromagnetic emf increased quadratically on increase in the magnetic field. An investigation was made of the barrier radiation-voltaic effect (when the emf was measured between the irradiated and unirradiated surfaces). Special masks were used to produce a set of consecutive p-n junctions in germanium crystals irradiated with α particles. A study of the photovoltaic and photoelectromagnetic effects in such samples showed that the method could be used to increase the efficiency of devices utilizing the photoelectromagnetic effect

  10. Crystallization of low saturated lipid blends of palm and canola oils with sorbitan monostearate and fully hydrogenated palm oil.

    Science.gov (United States)

    Barbosa, Karina Martins; Cardoso, Lisandro Pavie; Ribeiro, Ana Paula Badan; Kieckbusch, Theo Guenter; Buscato, Monise Helen Masuchi

    2018-03-01

    Several scientific investigations have focused on providing new strategies for supporting the development of low saturated and zero trans lipid materials, as healthier fat alternatives for food application. This work evaluated the consistency, crystallization behavior, microstructure and polymorphism of six blends composed of palm and canola oils at different concentrations (100:0, 80:20, 60:40, 40:60, 20:80 and 0:100, in w/w%) added with 5.0% of fully hydrogenated palm oil (FHPO) or with a mixture of 2.5% of FHPO and 2.5% of sorbitan monostearate (SMS). The results were compared with the non-structured blends (standard samples). Through microstructure images, the formation of a more homogeneous and denser packed crystal network was observed for samples added with both crystallization modifiers (FHPO/SMS) compared to the corresponding standard samples, after stabilization at 25 °C during 3 h. In particular, enhanced crystallization modifications were observed for the 40:60 blend, in which the crystal form β' emerged after the addition of FHPO/SMS. Moreover, the 40:60 blend structured with FHPO/SMS showed increased consistency (from 30 to 658 g F /cm 2 ) and induced onset crystallization in a higher temperature (from 13.1 to 23.9 °C) compared with the non-structured one, due to the specific crystallization effects provided by both added structurants.

  11. Influence of magnetic field on the morphology of the andrographolide crystal from supercritical carbon dioxide extraction crystallization

    Science.gov (United States)

    Chen, Kexun; Zhang, Xingyuan; Pan, Jian; Zhang, Wencheng; Yong, Ji; Yin, Wenhong

    2003-10-01

    In this paper, a supercritical fluid extraction-crystallization of andrographolide, a kind of Chinese traditional medicine, was investigated. We have studied the extraction-crystallization process with or without magnet in the extractor, respectively. It was found that the presence of magnetic field is an important factor influencing the quality of the products. SEM images showed that the crystal was slice-like in shape, and many slices reunited together in the absence of magnet. Further research showed that pressure had a certain effect on the morphology of the crystal.

  12. Monoolein lipid phases as incorporation and enrichment materials for membrane protein crystallization.

    Directory of Open Access Journals (Sweden)

    Ellen Wallace

    Full Text Available The crystallization of membrane proteins in amphiphile-rich materials such as lipidic cubic phases is an established methodology in many structural biology laboratories. The standard procedure employed with this methodology requires the generation of a highly viscous lipidic material by mixing lipid, for instance monoolein, with a solution of the detergent solubilized membrane protein. This preparation is often carried out with specialized mixing tools that allow handling of the highly viscous materials while minimizing dead volume to save precious membrane protein sample. The processes that occur during the initial mixing of the lipid with the membrane protein are not well understood. Here we show that the formation of the lipidic phases and the incorporation of the membrane protein into such materials can be separated experimentally. Specifically, we have investigated the effect of different initial monoolein-based lipid phase states on the crystallization behavior of the colored photosynthetic reaction center from Rhodobacter sphaeroides. We find that the detergent solubilized photosynthetic reaction center spontaneously inserts into and concentrates in the lipid matrix without any mixing, and that the initial lipid material phase state is irrelevant for productive crystallization. A substantial in-situ enrichment of the membrane protein to concentration levels that are otherwise unobtainable occurs in a thin layer on the surface of the lipidic material. These results have important practical applications and hence we suggest a simplified protocol for membrane protein crystallization within amphiphile rich materials, eliminating any specialized mixing tools to prepare crystallization experiments within lipidic cubic phases. Furthermore, by virtue of sampling a membrane protein concentration gradient within a single crystallization experiment, this crystallization technique is more robust and increases the efficiency of identifying productive

  13. Development of paracetamol-caffeine co-crystals to improve compressional, formulation and in vivo performance.

    Science.gov (United States)

    Latif, Sumera; Abbas, Nasir; Hussain, Amjad; Arshad, Muhammad Sohail; Bukhari, Nadeem Irfan; Afzal, Hafsa; Riffat, Sualeha; Ahmad, Zeeshan

    2018-07-01

    Paracetamol, a frequently used antipyretic and analgesic drug, has poor compression moldability owing to its low plasticity. In this study, new co-crystals of paracetamol (PCM) with caffeine (as a co-former) were prepared and delineated. Co-crystals exhibited improved compaction and mechanical behavior. A screening study was performed by utilizing a number of methods namely dry grinding, liquid assisted grinding (LAG), solvent evaporation (SE), and anti-solvent addition using various weight ratios of starting materials. LAG and SE were found successful in the screening study. Powders at 1:1 and 2:1 weight ratio of PCM/CAF by LAG and SE, respectively, resulted in the formation of co-crystals. Samples were characterized by PXRD, DSC, and ATR-FTIR techniques. Compressional properties of PCM and developed co-crystals were analyzed by in-die heckle model. Mean yield pressure (Py), an inverse measure of plasticity, obtained from the heckle plots decreased significantly (p < .05) for co-crystals than pure drug. Intrinsic dissolution profile of co-crystals showed up to 2.84-fold faster dissolution than PCM and physical mixtures in phosphate buffer pH 6.8 at 37 °C. In addition, co-crystals formulated into tablets by direct compression method showed better mechanical properties like hardness and tensile strength. In vitro dissolution studies on tablets also showed enhanced dissolution profiles (∼90-97%) in comparison to the tablets of PCM prepared by direct compression (∼55%) and wet granulation (∼85%) methods. In a single dose sheep model study, co-crystals showed up to twofold increase in AUC and C max . A significant (p < .05) decrease in clearance as compared to pure drug was also recorded. In conclusion, new co-crystals of PCM were successfully prepared with improved tabletability in vitro and in vivo profile. Enhancement in AUC and C max of PCM by co-crystallization might suggest the dose reduction and avoidance of side effects.

  14. Crystal and electronic structure study of Mn doped wurtzite ZnO nanoparticles

    Directory of Open Access Journals (Sweden)

    O.M. Ozkendir

    2016-08-01

    Full Text Available The change in the crystal and electronic structure properties of wurtzite ZnO nanoparticles was studied according to Mn doping in the powder samples. The investigations were conducted by X-ray Absorption Fine Structure Spectroscopy (XAFS technique for the samples prepared with different heating and doping processes. Electronic analysis was carried out by the collected data from the X-ray Absorption Near-Edge Structure Spectroscopy (XANES measurements. Additional crystal structure properties were studied by Extended-XAFS (EXAFS analysis. Longer heating periods for the undoped wurtzite ZnO samples were determined to own stable crystal geometries. However, for some doped samples, the distortions in the crystal were observed as a result of the low doping amounts of Mn which was treated as an impurity. Besides, the changes in oxygen locations were determined to create defects and distortions in the samples.

  15. Crystal structure and spin state of mixed-crystals of iron with NCS and NCBH3 for the assembled complexes bridged by 1,3-bis(4-pyridyl)propanes

    International Nuclear Information System (INIS)

    Haruka Dote; Hiroki Yasuhara

    2015-01-01

    New mixed crystals, Fe(NCS) x (NCBH 3 )( 2-x )(bpp) 2 , (bpp = 1,3-bis(4-pyridyl)propane) were synthesized. The formation of mixed crystals was confirmed by powder X-ray diffraction patterns and single crystal X-ray structural analysis. Elemental analyses showed that all Fe(NCS) x (NCBH 3 )( 2-x )(bpp) 2 samples had more Fe(NCS) 2 unit than the preparation fraction. 57 Fe Moessbauer spectroscopy revealed that all the spectra consist of only Fe(NCS) 2 unit and Fe(NCBH 3 ) 2 unit. And the fraction of low-spin state in the Fe(NCBH 3 ) 2 unit changed with the change of x. The results suggested that the high spin site of Fe(NCS) 2 unit affects the spin state of Fe(NCBH 3 ) 2 unit. (author)

  16. Improvement of several properties of lead tungstate crystals with different doping ions

    CERN Document Server

    Auffray, Etiennette; Baccaro, Stefania; Cecilia, Angelica; Dafinei, Ioan; Diemoz, Marcella; Jarolímek, O; Korzhik, Mikhail; Lecoq, Paul; Nikl, M

    1998-01-01

    A very good radiation resistance of Lead Tungstate crystals is mandatory for their use in the high precision electromagnetic calorimeter of the CMS experiment at LHC. Since the beginning of 1996 we have organised systematic investigations of the parameters influencing the radiation hardness of this crystal. Two classes of parameters have been particularly studied, the first one related to the control of the stoichiometry and structure associated defects, the second one connected with the suppression and the charge compensation of existing defects with different kinds of doping ions. This paper reports about the second part of this study and complements a first paper where the role of the stoichiometry was already discussed. Results of tests are given on a significant statistical sample of full size crystals ( 23cm) which show a considerable improvement in the optical properties and the radiation resistance of appropriately doped crystals.

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

    International Nuclear Information System (INIS)

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

    1988-01-01

    High-quality single crystals of Bi 2 CaSr 2 Cu 2 O 8 superconductors have been prepared and cleaved in ultrahigh vacuum. Low-energy electron diffraction measurements show that the surface structure is consistent with the bulk crystal structure. Ultraviolet photoemission and x-ray photoemission experiments were performed on these well-characterized sample surfaces. The valence-band and the core-level spectra obtained from the single-crystal surfaces are in agreement with spectra recorded from polycrystalline samples, justifying earlier results from polycrystalline samples. Cu satellites are observed both in the valence band and Cu 2p core level, signaling the strong correlation among the Cu 3d electrons. The O 1s core-level data exhibit a sharp, single peak at 529-eV binding energy without any clear satellite structures

  18. Low Leakage Superconducting Tunnel Junctions with a Single Crystal Al2O3 Barrier

    Science.gov (United States)

    2016-03-30

    10-6 Torr ). In this low-pressure oxygen environment, Auger electron spectroscopy (AES) study shows that while oxidation of the base layer is...three layers were grown in situ in an ultra high vacuum (UHV) system with a nominal base pressure of ~1×10-10 Torr . First, a 120~150 nm thick...high-temperature annealing in order to crystallize the amorphous AlOx into a single-crystal Al2O3. After the sample was cooled to room temperature

  19. Primary and aggregate color centers in proton irradiated LiF crystals and thin films for luminescent solid state detectors

    Science.gov (United States)

    Piccinini, M.; Ambrosini, F.; Ampollini, A.; Bonfigli, F.; Libera, S.; Picardi, L.; Ronsivalle, C.; Vincenti, M. A.; Montereali, R. M.

    2015-04-01

    Proton beams of 3 MeV energy, produced by the injector of a linear accelerator for proton therapy, were used to irradiate at room temperature lithium fluoride crystals and polycrystalline thin films grown by thermal evaporation. The irradiation fluence range was 1011-1015 protons/cm2. The proton irradiation induced the stable formation of primary and aggregate color centers. Their formation was investigated by optical absorption and photoluminescence spectroscopy. The F2 and F3+ photoluminescence intensities, carefully measured in LiF crystals and thin films, show linear behaviours up to different maximum values of the irradiation fluence, after which a quenching is observed, depending on the nature of the samples (crystals and films). The Principal Component Analysis, applied to the absorption spectra of colored crystals, allowed to clearly identify the formation of more complex aggregate defects in samples irradiated at highest fluences.

  20. Single-crystal growth of ceria-based materials; Einkristallzuechtung von Materialien auf der Basis von Cerdioxid

    Energy Technology Data Exchange (ETDEWEB)

    Ulbrich, Gregor

    2015-07-23

    In this work it could be shown that Skull-Melting is a suitable method for growing ceria single crystals. Twenty different ceria-based single crystals could be manufactured. It was possible to dope ceria single crystals with Gd, Sm, Y, Zr, Ti, Ta, and Pr in different concentrations. Also co-doping with the named metals was realized. However, there remain some problems for growing ceria-based single crystals by Skull-Melting. As ignition metal zirconium was used because no ceria-based material works well. For that reason all single crystals show small zirconium contamination. Another problem is the formation of oxygen by the heat-induced reduction of ceria during the melting process. Because of that the skull of sintered material is often destroyed by gas pressure. This problem had to be solved individually for every single crystal. The obtained single crystals were characterized using different methods. To ensure the single crystal character the y were examined by Laue diffraction. All manufactured crystals are single crystals. Also powder diffraction patterns of the milled and oxidized samples were measured. For the determination of symmetry and metric the structural parameters were analyzed by the Rietveld method. All synthesized materials crystallize in space group Fm-3m known from calcium fluoride. The cubic lattice parameter a was determined for all crystals. In the case of series with different cerium and zirconium concentrations a linear correlation between cerium content and cubic lattice parameter was detected. The elemental composition was determined by WDX. All crystals show a homogeneous elemental distribution. The oxygen content was calculated because the WDX method isn't useful for determination.

  1. Sound absorption enhancement of nonwoven felt by using coupled membrane - sonic crystal inclusion

    Science.gov (United States)

    Fitriani, M. C.; Yahya, I.; Harjana; Ubaidillah; Aditya, F.; Siregar, Y.; Moeliono, M.; Sulaksono, S.

    2016-11-01

    The experimental results from laboratory test on the sound absorption performance of nonwoven felt with an array thin tubes and sonic crystal inclusions reported in this paper. The nonwoven felt sample was produced by a local company with 15 mm in its thickness and 900 gsm. The 6.4 mm diameter plastic straw was used to construct the thin tubes array while the sonic crystal is arranged in a 4 × 4 lattice crystal formation. It made from a PVC cylinder with 17 mm and 50 mm in diameter and length respectively. All cylinders have two holes positioned on 10 mm and 25 mm from the base. The results show that both treatments, array of thin tube and sonic crystal inclusions are effectively increased the sound absorption coefficient of the nonwoven felt significantly especially in the low frequency range starting from 200Hz.

  2. Application of Micro-cloud point extraction for spectrophotometric determination of Malachite green, Crystal violet and Rhodamine B in aqueous samples

    Science.gov (United States)

    Ghasemi, Elham; Kaykhaii, Massoud

    2016-07-01

    A novel, green, simple and fast method was developed for spectrophotometric determination of Malachite green, Crystal violet, and Rhodamine B in water samples based on Micro-cloud Point extraction (MCPE) at room temperature. This is the first report on the application of MCPE on dyes. In this method, to reach the cloud point at room temperature, the MCPE procedure was carried out in brine using Triton X-114 as a non-ionic surfactant. The factors influencing the extraction efficiency were investigated and optimized. Under the optimized condition, calibration curves were found to be linear in the concentration range of 0.06-0.60 mg/L, 0.10-0.80 mg/L, and 0.03-0.30 mg/L with the enrichment factors of 29.26, 85.47 and 28.36, respectively for Malachite green, Crystal violet, and Rhodamine B. Limit of detections were between 2.2 and 5.1 μg/L.

  3. Crystallization of glycine with ultrasound

    DEFF Research Database (Denmark)

    Louhi-Kultanen, Marjatta; Karjalainen, Milja; Rantanen, Jukka

    2006-01-01

    Sonocrystallization has proved to be an efficient tool to influence the external appearance and structure of a crystalline product obtained by various crystallization methods. The present work focuses on high intensity sonocrystallization of glycine by varying amplitude of ultrasound with an ultr...... ultrasound power. This study also showed, the higher the ultrasound amplitude the smaller the crystals obtained.......Sonocrystallization has proved to be an efficient tool to influence the external appearance and structure of a crystalline product obtained by various crystallization methods. The present work focuses on high intensity sonocrystallization of glycine by varying amplitude of ultrasound...... with an ultrasound frequency of 20kHz at two temperature ranges 40-50 and 20-30 degrees C in a jacketed 250-ml cooling crystallizer equipped with a stirrer. The polymorph composition of the obtained crystals was analyzed with a temperature variable X-ray powder diffractometer (XRPD). XRPD results showed that...

  4. Growth and characterization of nonlinear optical bimetallic thiocyanate complex of MCCTC crystal

    Science.gov (United States)

    Ravi Kumar, S. M.; Melikechi, N.; Selvakumar, S.; Sagayaraj, P.

    2009-04-01

    An organometallic material of mercury cadmium chloride thiocyanate (MCCTC) was synthesized in water-methanol mixed solvent. Optically good grade crystal was grown by slow evaporation technique under optimized conditions. MCCTC belongs to rhombohedral system with R3c space group. The metal coordinations with (S with Hg and N with Cd) SCN - ion were confirmed in the sample by Fourier transform infrared (FT-IR) spectroscopic investigations. The transmission spectrum recorded from 200 to 2500 nm showed the UV transparency cutoff at 300 nm. MCCTC crystal exhibits a second-harmonic generation (SHG) efficiency which is nearly 17 times more than that of KDP. The microhardness study indicates the hard nature of the grown sample with a work hardening coefficient of 1.73. The thermal decomposition process was investigated by thermo gravimetric and differential thermal analyses.

  5. Study of thermochemically reduced and electron-irradiated LiNbO3 single crystals by positron annihilation and optical absorption measurements

    International Nuclear Information System (INIS)

    Pareja, R.; Gonzalez, R.; Pedrosa, M.A.

    1984-01-01

    Irradiation of LiNbO 3 single crystals using Van de Graaff electrons with an energy of 1.5 MeV introduces an optical absorption band similar to that observed in thermochemically reduced samples. As-grown, reduced, or irradiated crystals show single-component positron lifetime spectra with an average decay time of 234 ps. (author)

  6. Crystal structures of superconducting sodium intercalates of hafnium nitride chloride

    International Nuclear Information System (INIS)

    Oro-Sole, J.; Frontera, C.; Beltran-Porter, D.; Lebedev, O.I.; Van Tendeloo, G.; Fuertes, A.

    2006-01-01

    Sodium intercalation compounds of HfNCl have been prepared at room temperature in naphtyl sodium solutions in tetrahydrofuran and their crystal structure has been investigated by Rietveld refinement using X-ray powder diffraction data and high-resolution electron microscopy. The structure of two intercalates with space group R3-bar m and lattice parameters a=3.58131(6)A, c=57.752(6)A, and a=3.58791(8)A, c=29.6785(17)A is reported, corresponding to the stages 2 and 1, respectively, of Na x HfNCl. For the stage 2 phase an ordered model is presented, showing two crystallographically independent [HfNCl] units with an alternation of the Hf-Hf interlayer distance along the c-axis, according with the occupation by sodium atoms of one out of two van der Waals gaps. Both stages 1 and 2 phases are superconducting with critical temperatures between 20 and 24K, they coexist in different samples with proportions depending on the synthesis conditions, and show a variation in c spacing that can be correlated with the sodium stoichiometry. High-resolution electron microscopy images of the host and intercalated samples show bending of the HfNCl bilayers as well as stacking faults in some regions, which coexist in the same crystal with ordered domains

  7. Crystallization, optimization and preliminary X-ray characterization of a metal-dependent PI-PLC from Streptomyces antibioticus

    International Nuclear Information System (INIS)

    Jackson, Michael R.; Selby, Thomas L.

    2012-01-01

    Crystallization and diffraction analysis of a Ca 2+ -dependent PI-PLC from Streptomyces is reported. Optimization of crystals was completed using a drop-pinning technique and heavy-atom soaks to achieve high-quality diffraction to 1.23 Å. A recombinant metal-dependent phosphatidylinositol-specific phospholipase C (PI-PLC) from Streptomyces antibioticus has been crystallized by the hanging-drop method with and without heavy metals. The native crystals belonged to the orthorhombic space group P222, with unit-cell parameters a = 41.26, b = 51.86, c = 154.78 Å. The X-ray diffraction results showed significant differences in the crystal quality of samples soaked with heavy atoms. Additionally, drop pinning, which increases the surface area of the drops, was also used to improve crystal growth and quality. The combination of heavy-metal soaks and drop pinning was found to be critical for producing high-quality crystals that diffracted to 1.23 Å resolution

  8. Graded photonic crystals by optical interference holography

    International Nuclear Information System (INIS)

    Han, Chunrui; Tam, Wing Yim

    2012-01-01

    We report on the fabrication of graded photonic crystals in dye doped dichromate gelatin emulsions using an optical interference holographic technique. The gradedness is achieved by imposing a gradient form factor in the interference intensity resulting from the absorption of the dye in the dichromate gelatin. Wider and deeper photonic bandgaps are observed for the dyed samples as compared to the un-dyed samples. Our method could open up a new direction in fabricating graded photonic crystals which cannot be achieved easily using other techniques. (paper)

  9. Structural, mechanical and light yield characterisation of heat treated LYSO:Ce single crystals for medical imaging applications

    CERN Document Server

    Mengucci, P; Auffray, E; Barucca, G; Cecchi, C; Chipaux, R; Cousson, A; Davì, F; Di Vara, N; Rinaldi, D; Santecchia, E

    2015-01-01

    Five single crystals of cerium-doped lutetium yttrium oxyorthosilicate (LYSO:Ce) grown by the Czochralski method were submitted to structural characterisation by X-ray (XRD) and neutron (ND) diffraction, scanning (SEM) and transmission (TEM) electron microscopy and energy dispersive microanalysis (EDS). The Ultimate Tensile Strength (UTS), the Young Modulus (YM) and the Light Yield (LY) of the samples were also measured in order to correlate the mechanical and the optical behaviour of the crystals with the characteristics of their microstructure. Two of the samples analysed were also heat treated at 300 °C for 10 h to evidence possible variations induced by the temperature in the optical and mechanical response of the crystals. Results showed that the mean compositional variations evidenced by the structural analyses do not affect the mechanical and optical behaviour of the samples. On the contrary, the thermal treatment could induce the formation of coherent spherical particles (size 10 to 15 nm), not unifo...

  10. Optical Study of Liquid Crystal Doped with Multiwalled Carbon Nanotube

    Science.gov (United States)

    Gharde, Rita A.; Thakare, Sangeeta Y.

    2014-11-01

    Liquid crystalline materials have been useful for display devices i.e watches, calculators, automobile dashboards, televisions, multi media projectors etc. as well as in electro tunable lasers, optical fibers and lenses. Carbon nanotube is chosen as the main experimental factor in this study as it has been observed that Carbon Nano Tube influence the existing properties of liquid crystal host and with the doping of CNT can enhance1 the properties of LC. The combination of carbon nanotube (CNT) and liquid crystal (LC) materials show considerable interest in the scientific community due to unique physical properties of CNT in liquid crystal. Dispersion of CNTs in LCs can provide us a cheap, simple, versatile and effective means of controlling nanotube orientation on macroscopic scale with no restrictions on nanotube type. LCs have the long range orientational order rendering them to be anisotropic phases. If CNTs can be well dispersed in LC matrix, they will align with their long axes along the LC director to minimize distortions of the LC director field and the free energy. In this paper, we doped liquid crystal (Cholesteryl Nonanoate) by a small amount of multiwall carbon nanotube 0.05% and 0.1% wt. We found that by adding carbon nanotube to liquid crystals the melting point of the mixture is decreased but TNI is increased. It has been also observed that with incereas in concentration of carbon nanotube into liquid crystal shows conciderable effect on LC. The prepared samples were characterized using various techniques to study structural, thermal and optical properties i.e PMS, FPSS, UV-Vis spectroscopy, FT-IR measurements, and DTA.

  11. Growth, structural and magnetic characterization of Al-substituted barium hexaferrite single crystals

    International Nuclear Information System (INIS)

    Vinnik, D.A.; Zherebtsov, D.A.; Mashkovtseva, L.S.; Nemrava, S.; Bischoff, M.; Perov, N.S.; Semisalova, A.S.; Krivtsov, I.V.; Isaenko, L.I.; Mikhailov, G.G.; Niewa, R.

    2014-01-01

    Highlights: • Growth of large Al-substituted crystals BaFe 12−x Al x O 19. • Al-content controllable by flux composition. • Crystallographic site preference of Al unraveled. • Magnetic characterization depending on Al-content. - Abstract: Large single crystals of aluminum-substituted M-type barium hexaferrite BaFe 12−x Al x O 19 were obtained from carbonate flux. The Al content in the crystals can be controlled via the Al content of the flux up to x = 1.1 according to single crystal X-ray structure refinements. Al shows a distinct preference to substitute Fe on crystallographic sites with high coordination numbers by oxygen atoms, whereas no significant amounts of Al can be found on a tetrahedrally coordinated site. An increasing amount of the aluminum dopant results in a monotonous reduction of the Curie temperature from 440 to 415 °C and the saturation magnetization at room temperature from 68 to 57 emu/g for single crystal and from 61 to 53 emu/g for powder samples

  12. Growth and characterizaion of urea p-nitrophenol crystal: an organic nonlinear optical material for optoelectronic device application

    Science.gov (United States)

    Suresh, A.; Manikandan, N.; Jauhar, RO. MU.; Murugakoothan, P.; Vinitha, G.

    2018-06-01

    Urea p-nitrophenol, an organic nonlinear optical crystal was synthesized and grown adopting slow evaporation and seed rotation method. Single crystal X-ray diffraction study confirmed the formation of the desired crystal. High resolution X-ray diffraction study showed the defect nature of the crystal. The presence of functional groups in the material was confirmed by FTIR analysis. UV-Vis-NIR study indicates that the grown crystal has a wider transparency region with the lower cutoff wavelength at 423 nm. The grown crystal is thermally stable up to 120 °C as assessed by TG-DTA analysis. The optical homogeneity of the grown crystal was confirmed by birefringence study. The 1064 nm Nd-YAG laser was used to obtain laser induced surface damage threshold which was found to be 0.38, 0.25 and 0.33 GW/cm2 for (0 1 0), (1 1 - 1) and (0 1 1) planes, respectively. The dielectric study was performed to find the charge distribution inside the crystal. The hardness property of the titular material has been found using Vicker's microhardness study. The optical nonlinearity obtained from third order nonlinear optical measurements carried out using Z-scan technique showed that these samples could be exploited for optical limiting studies.

  13. Conformation of comb liquid crystal polymers by neutron small angle scattering

    International Nuclear Information System (INIS)

    Noirez, L.; Pepy, G.

    1988-01-01

    A review is made of the direct information obtained by small angle neutron scattering about the anisotropy of the components parallel and perpendicular to the orienting magnetic field of the radius of gyration of comb like liquid crystal polymers. The behaviour of the conformation versus temperature is reported for several samples. Until now all samples show an oblate conformation in the smectic phase and probably the whole range of the nematic phase. The results are compared with the available theoretical predictions

  14. Magnetic, transport, and optical properties of Ca{sub 0.85}Eu{sub 0.15}MnO{sub 3} single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Naumov, S.V., E-mail: naumov@imp.uran.ru [Institute of Metal Physics, Ural Branch of RAS, Kovalevskaya Street 18, Ekaterinburg 620990 (Russian Federation); Loshkareva, N.N.; Mostovshchikova, E.V.; Solin, N.I.; Korolev, A.V.; Arbuzova, T.I.; Telegin, S.V.; Patrakov, E.I. [Institute of Metal Physics, Ural Branch of RAS, Kovalevskaya Street 18, Ekaterinburg 620990 (Russian Federation)

    2013-01-01

    Magnetic, transport and optical properties of the Ca{sub 0.85}Eu{sub 0.15}MnO{sub 3} single crystal are studied and discussed in comparison with the properties of polycrystalline sample. The magnetic data show existence the two magnetic phase transitions under cooling: the transition near 150 K occurs from the paramagnetic orthorhombic to C-type antiferromagnetic monoclinic phase with the charge/orbital ordering in some part of the crystal; and at 90 K the transition from the paramagnetic to G-type antiferromagnetic phase takes place in another part of the crystal with the orthorhombic structure. The magnetoresistance of the Ca{sub 0.85}Eu{sub 0.15}MnO{sub 3} single crystal has features at temperatures of these phase transitions. Differences in the properties of single crystal and polycrystalline sample with the same content of Eu are associated with the ordering of oxygen vacancies that appear under the crystal growth. The reflection spectra in infrared range confirm the existence of the electron conductivity in a narrow band at room temperature.

  15. Effect of Different Crystallization Techniques on the Dissolution ...

    African Journals Online (AJOL)

    HP

    Methods: Ketoprofen crystals were prepared by various crystallization technique including spherical .... infrared. (FTIR) spectroscopy. FTIR spectral measurements were taken at ambient temperature (Shimadzu, model 8033,. USA). About 2 mg of the pure drug, as well as ... stored samples and the data compared with.

  16. Density-viscosity product of small-volume ionic liquid samples using quartz crystal impedance analysis.

    Science.gov (United States)

    McHale, Glen; Hardacre, Chris; Ge, Rile; Doy, Nicola; Allen, Ray W K; MacInnes, Jordan M; Bown, Mark R; Newton, Michael I

    2008-08-01

    Quartz crystal impedance analysis has been developed as a technique to assess whether room-temperature ionic liquids are Newtonian fluids and as a small-volume method for determining the values of their viscosity-density product, rho eta. Changes in the impedance spectrum of a 5-MHz fundamental frequency quartz crystal induced by a water-miscible room-temperature ionic liquid, 1-butyl-3-methylimiclazolium trifluoromethylsulfonate ([C4mim][OTf]), were measured. From coupled frequency shift and bandwidth changes as the concentration was varied from 0 to 100% ionic liquid, it was determined that this liquid provided a Newtonian response. A second water-immiscible ionic liquid, 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide [C4mim][NTf2], with concentration varied using methanol, was tested and also found to provide a Newtonian response. In both cases, the values of the square root of the viscosity-density product deduced from the small-volume quartz crystal technique were consistent with those measured using a viscometer and density meter. The third harmonic of the crystal was found to provide the closest agreement between the two measurement methods; the pure ionic liquids had the largest difference of approximately 10%. In addition, 18 pure ionic liquids were tested, and for 11 of these, good-quality frequency shift and bandwidth data were obtained; these 12 all had a Newtonian response. The frequency shift of the third harmonic was found to vary linearly with square root of viscosity-density product of the pure ionic liquids up to a value of square root(rho eta) approximately 18 kg m(-2) s(-1/2), but with a slope 10% smaller than that predicted by the Kanazawa and Gordon equation. It is envisaged that the quartz crystal technique could be used in a high-throughput microfluidic system for characterizing ionic liquids.

  17. Crystal nuclei templated nanostructured membranes prepared by solvent crystallization and polymer migration

    Science.gov (United States)

    Wang, Bo; Ji, Jing; Li, Kang

    2016-09-01

    Currently, production of porous polymeric membranes for filtration is predominated by the phase-separation process. However, this method has reached its technological limit, and there have been no significant breakthrough over the last decade. Here we show, using polyvinylidene fluoride as a sample polymer, a new concept of membrane manufacturing by combining oriented green solvent crystallization and polymer migration is able to obtain high performance membranes with pure water permeation flux substantially higher than those with similar pore size prepared by conventional phase-separation processes. The new manufacturing procedure is governed by fewer operating parameters and is, thus, easier to control with reproducible results. Apart from the high water permeation flux, the prepared membranes also show excellent stable flux after fouling and superior mechanical properties of high pressure load and better abrasion resistance. These findings demonstrate the promise of a new concept for green manufacturing nanostructured polymeric membranes with high performances.

  18. Manufacturing Amorphous Solid Dispersions with a Tailored Amount of Crystallized API for Biopharmaceutical Testing.

    Science.gov (United States)

    Theil, Frank; Milsmann, Johanna; Anantharaman, Sankaran; van Lishaut, Holger

    2018-05-07

    The preparation of an amorphous solid dispersion (ASD) by dissolving a poorly water-soluble active pharmaceutical ingredient (API) in a polymer matrix can improve the bioavailability by orders of magnitude. Crystallization of the API in the ASD, though, is an inherent threat for bioavailability. Commonly, the impact of crystalline API on the drug release of the dosage form is studied with samples containing spiked crystallinity. These spiked samples possess implicit differences compared to native crystalline samples, regarding size and spatial distribution of the crystals as well as their molecular environment. In this study, we demonstrate that it is possible to grow defined amounts of crystalline API in solid dosage forms, which enables us to study the biopharmaceutical impact of actual crystallization. For this purpose, we studied the crystal growth in fenofibrate tablets over time under an elevated moisture using transmission Raman spectroscopy (TRS). As a nondestructive method to assess API crystallinity in ASD formulations, TRS enables the monitoring of crystal growth in individual dosage forms. Once the kinetic trace of the crystal growth for a certain environmental condition is determined, this method can be used to produce samples with defined amounts of crystallized API. To investigate the biopharmaceutical impact of crystallized API, non-QC dissolution methods were used, designed to identify differences between the various amounts of crystalline materials present. The drug release in the samples manufactured in this fashion was compared to that of samples with spiked crystallinity. In this study, we present for the first time a method for targeted crystallization of amorphous tablets to simulate crystallized ASDs. This methodology is a valuable tool to generate model systems for biopharmaceutical studies on the impact of crystallinity on the bioavailability.

  19. Strengthening mechanisms of Fe nanoparticles for single crystal Cu–Fe alloy

    International Nuclear Information System (INIS)

    Shi, Guodong; Chen, Xiaohua; Jiang, Han; Wang, Zidong; Tang, Hao; Fan, Yongquan

    2015-01-01

    A single crystal Cu–Fe alloy with finely dispersed precipitate Fe nanoparticles was fabricated in this study. The interface relationship of iron nanoparticle and copper matrix was analyzed with a high-resolution transmission electron microscope (HRTEM), and the effect of Fe nanoparticles on mechanical properties of single crystal Cu–Fe alloy was discussed. Results show that, the finely dispersed Fe nanoparticles can be obtained under the directional solidification condition, with the size of 5–50 nm and the coherent interface between the iron nanoparticle and the copper matrix. Single crystal Cu–Fe alloy possesses improved tensile strength of 194.64 MPa, and total elongation of 44.72%, respectively, at room temperature, in contrast to pure Cu sample. Nanoparticles which have coherent interface with matrix can improve the dislocation motion state. Some dislocations can slip through the nanoparticle along the coherent interface and some dislocations can enter into the nanoparticles. Thus to improve the tensile strength of single crystal Cu–Fe alloy without sacrificing the ductility simultaneously. Based on the above analyses, strengthening mechanisms of Fe nanoparticles for single crystal Cu–Fe alloy was described

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

    Energy Technology Data Exchange (ETDEWEB)

    Warren, Anna J. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom); Crawshaw, Adam D. [Newcastle University, Newcastle upon Tyne NE2 4HH (United Kingdom); Trincao, Jose; Aller, Pierre; Alcock, Simon; Nistea, Ioana [Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom); Salgado, Paula S. [Newcastle University, Newcastle upon Tyne NE2 4HH (United Kingdom); Evans, Gwyndaf, E-mail: gwyndaf.evans@diamond.ac.uk [Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom)

    2015-09-26

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  2. Crystal modifications and dissolution rate of piroxicam.

    Science.gov (United States)

    Lyn, Lim Yee; Sze, Huan Wen; Rajendran, Adhiyaman; Adinarayana, Gorajana; Dua, Kamal; Garg, Sanjay

    2011-12-01

    Piroxicam is a nonsteroidal anti-inflammatory drug with low aqueous solubility which exhibits polymorphism. The present study was carried out to develop polymorphs of piroxicam with enhanced solubility and dissolution rate by the crystal modification technique using different solvent mixtures prepared with PEG 4000 and PVP K30. Physicochemical characteristics of the modified crystal forms of piroxicam were investigated by X-ray powder diffractometry, FT-IR spectrophotometry and differential scanning calorimetry. Dissolution and solubility profiles of each modified crystal form were studied and compared with pure piroxicam. Solvent evaporation method (method I) produced both needle and cubic shaped crystals. Slow crystallization from ethanol with addition of PEG 4000 or PVP K30 at room temperature (method II) produced cubic crystal forms. Needle forms produced by method I improved dissolution but not solubility. Cubic crystals produced by method I had a dissolution profile similar to that of untreated piroxicam but showed better solubility than untreated piroxicam. Cubic shaped crystals produced by method II showed improved dissolution, without a significant change in solubility. Based on the XRPD results, modified piroxicam crystals obtained by method I from acetone/benzene were cube shaped, which correlates well with the FTIR spectrum; modified needle forms obtained from ethanol/methanol and ethanol/acetone showed a slight shift of FTIR peak that may be attributed to differences in the internal structure or conformation.

  3. Further results on cerium fluoride crystals

    International Nuclear Information System (INIS)

    Anderson, S.; Auffray, E.; Aziz, T.; Baccaro, S.; Banerjee, S.; Bareyre, P.; Barone, L.E.; Borgia, B.; Boutet, D.; Burq, J.P.; Chemarin, M.; Chipaux, R.; Dafinei, I.; D'Atanasio, P.; De Notaristefani, F.; Dezillie, B.; Dujardin, C.; Dutta, S.; Faure, J.L.; Fay, J.; Ferrere, D.; Francescangeli, O.; Fuchs, B.A.; Ganguli, S.N.; Gillespie, G.; Goyot, M.; Gupta, S.K.; Gurtu, A.; Heck, J.; Herve, A.; Hillemanns, H.; Holdener, F.; Ille, B.; Joensson, L.; Kierstead, J.; Krenz, W.; Kway, W.; Le Goff, J.M.; Lebeau, M.; Lebrun, P.; Lecoq, P.; Lemoigne, Y.; Loomis, G.; Lubelsmeyer, K.; Madjar, N.; Majni, G.; El Mamouni, H.; Mangla, S.; Mares, J.A.; Martin, J.P.; Mattioli, M.; Mauger, G.J.; Mazumdar, K.; Mengucci, P.; Merlo, J.P.; Moine, B.; Nikl, N.; Pansart, J.P.; Pedrini, C.; Poinsignon, J.; Polak, K.; Raghavan, R.; Rebourgeard, P.; Rinaldi, D.; Rosa, J.; Rosowsky, A.; Sahuc, P.; Samsonov, V.; Sarkar, S.; Schegelski, V.; Schmitz, D.; Schneegans, M.; Seliverstov, D.; Stoll, S.; Sudhakar, K.; Svensson, A.; Tonwar, S.C.; Topa, V.; Vialle, J.P.; Vivargent, M.; Wallraff, W.; Weber, M.J.; Winter, N.; Woody, C.; Wuest, C.R.; Yanovski, V.

    1993-01-01

    A systematic investigation of the properties of cerium fluoride monocrystals has been performed by the 'Crystal Clear' collaboration in view of a possible use of such crystals for the construction of high precision electromagnetic calorimeters for the future generation of high luminosity accelerators. A large sample of different crystals grown by several producers has been studied. The spectroscopic characteristics, the transmission, luminescence and excitation spectra and the decay time curves are analysed. The light yield of the different crystals is measured with photomultipliers and Si photodiodes and compared to reference standards like BGO and NaI(Tl). The radiation damage behaviour is then presented for γ and neutron irradiations, at different doses and dose rates, including thermal and optical bleaching. (orig.)

  4. Cooling Crystallization of Indomethacin: Effect of Supersaturation, Temperature and Seeding on Polymorphism and Crystal Size Distribution

    DEFF Research Database (Denmark)

    Malwade, Chandrakant Ramkrishna; Qu, Haiyan

    2018-01-01

    In this work, effect of crystallization parameters i.e., supersaturation, seeding, and temperature on polymorphism and crystal size of a non-steroidal anti-inflammatory drug, indomethacin (IMC), was investigated. Firstly, several crystallization solvents (ethanol, methanol, ethyl acetate, acetone...... of IMC from ethanol confirmed that the supersaturation, operating temperature and seeding does affect the polymorphism as well as crystal size distribution of IMC. Fine needle shaped crystals of metastable α-IMC were obtained at 5 °C with high supersaturation even in presence of γ-IMC seeds, while...... rhombic plates like crystals of thermodynamically stable γ-IMC were obtained in remaining experiments. The amount of seed loading only marginally influenced the crystal growth rate and median particle diameter (d50). Particle size analysis of crystals obtained showed bimodal distribution in all...

  5. Primary and aggregate color centers in proton irradiated LiF crystals and thin films for luminescent solid state detectors

    International Nuclear Information System (INIS)

    Piccinini, M; Ambrosini, F; Ampollini, A; Bonfigli, F; Libera, S; Picardi, L; Ronsivalle, C; Vincenti, M A; Montereali, R M

    2015-01-01

    Proton beams of 3 MeV energy, produced by the injector of a linear accelerator for proton therapy, were used to irradiate at room temperature lithium fluoride crystals and polycrystalline thin films grown by thermal evaporation. The irradiation fluence range was 10 11 -10 15 protons/cm 2 . The proton irradiation induced the stable formation of primary and aggregate color centers. Their formation was investigated by optical absorption and photoluminescence spectroscopy. The F 2 and F 3 + photoluminescence intensities, carefully measured in LiF crystals and thin films, show linear behaviours up to different maximum values of the irradiation fluence, after which a quenching is observed, depending on the nature of the samples (crystals and films). The Principal Component Analysis, applied to the absorption spectra of colored crystals, allowed to clearly identify the formation of more complex aggregate defects in samples irradiated at highest fluences. (paper)

  6. Zinc oxide crystal whiskers as a novel sorbent for solid-phase extraction of flavonoids.

    Science.gov (United States)

    Wang, Licheng; Shangguan, Yangnan; Hou, Xiudan; Jia, Yong; Liu, Shujuan; Sun, Yingxin; Guo, Yong

    2017-08-15

    As a novel solid-phase extraction material, zinc oxide crystal whiskers were used to extract flavonoid compounds and showed good extraction abilities. X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy and surface area/pore volume characterized the sorbent. The zinc oxide was packed into a solid-phase extraction micro-column and its extraction ability was evaluated by four model flavonoid compounds. The sample loading and elution parameters were optimized and the zinc oxide based analytical method for flavonoids was established. It showed that the method has wide linearities from 1 to 150μg/L and low limits of detection at 0.25μg/L. The relative standard deviations of a single column repeatability and column to column reproducibility were less than 6.8% and 10.6%. Several real samples were analyzed by the established method and satisfactory results were obtained. The interactions between flavonoids and zinc oxide were calculated and proved to be from the Van der Waals' forces between the 4p and 5d orbitals from zinc atom and the neighboring π orbitals from flavonoid phenyl groups. Moreover, the zinc oxide crystal whiskers showed good stability and could be reused more than 50 times under the operation conditions. This work proves that the zinc oxide crystal whiskers are a good candidate for flavonoids enrichment. Copyright © 2017. Published by Elsevier B.V.

  7. 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.

  8. Shape effect related to crystallographic orientation of deformation behavior in copper crystals

    International Nuclear Information System (INIS)

    Kim, K.H.; Chang, C.H.; Koo, Y.M.; MacDowell, A.A.

    1999-01-01

    The deformation behavior of pure copper single crystals has been investigated by scanning electron microscopy and synchrotron radiation using the in situ reflection Laue method. Two types of samples with the same orientation of tensile axes, but with different crystallographic orientations in the directions of the width and thickness of the samples, have been studied. They showed different characteristics of deformation behavior, such as the activated slip systems, the movement of the tensile axis, and the mode of fracture

  9. Large-surface-area diamond (111) crystal plates for applications in high-heat-load wavefront-preserving X-ray crystal optics.

    Science.gov (United States)

    Stoupin, Stanislav; Antipov, Sergey; Butler, James E; Kolyadin, Alexander V; Katrusha, Andrey

    2016-09-01

    Fabrication and results of high-resolution X-ray topography characterization of diamond single-crystal plates with large surface area (10 mm × 10 mm) and (111) crystal surface orientation for applications in high-heat-load X-ray crystal optics are reported. The plates were fabricated by laser-cutting of the (111) facets of diamond crystals grown using high-pressure high-temperature methods. The intrinsic crystal quality of a selected 3 mm × 7 mm crystal region of one of the studied samples was found to be suitable for applications in wavefront-preserving high-heat-load crystal optics. Wavefront characterization was performed using sequential X-ray diffraction topography in the pseudo plane wave configuration and data analysis using rocking-curve topography. The variations of the rocking-curve width and peak position measured with a spatial resolution of 13 µm × 13 µm over the selected region were found to be less than 1 µrad.

  10. Characterization of high level nuclear waste glass samples following extended melter idling

    Energy Technology Data Exchange (ETDEWEB)

    Fox, Kevin M. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Peeler, David K. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Kruger, Albert A. [USDOE Office of River Protection, Richland, WA (United States)

    2015-06-16

    The Savannah River Site Defense Waste Processing Facility (DWPF) melter was recently idled with glass remaining in the melt pool and riser for approximately three months. This situation presented a unique opportunity to collect and analyze glass samples since outages of this duration are uncommon. The objective of this study was to obtain insight into the potential for crystal formation in the glass resulting from an extended idling period. The results will be used to support development of a crystal-tolerant approach for operation of the high-level waste melter at the Hanford Tank Waste Treatment and Immobilization Plant (WTP). Two glass pour stream samples were collected from DWPF when the melter was restarted after idling for three months. The samples did not contain crystallization that was detectible by X-ray diffraction. Electron microscopy identified occasional spinel and noble metal crystals of no practical significance. Occasional platinum particles were observed by microscopy as an artifact of the sample collection method. Reduction/oxidation measurements showed that the pour stream glasses were fully oxidized, which was expected after the extended idling period. Chemical analysis of the pour stream glasses revealed slight differences in the concentrations of some oxides relative to analyses of the melter feed composition prior to the idling period. While these differences may be within the analytical error of the laboratories, the trends indicate that there may have been some amount of volatility associated with some of the glass components, and that there may have been interaction of the glass with the refractory components of the melter. These changes in composition, although small, can be attributed to the idling of the melter for an extended period. The changes in glass composition resulted in a 70-100 °C increase in the predicted spinel liquidus temperature (TL) for the pour stream glass samples relative to the analysis of the melter feed prior to

  11. Twinning processes in Cu-Al-Ni martensite single crystals investigated by neutron single crystal diffraction method

    International Nuclear Information System (INIS)

    Molnar, P.; Sittner, P.; Novak, V.; Lukas, P.

    2008-01-01

    A neutron single crystal diffraction method for inspecting the quality of martensite single crystals is introduced. True interface-free martensite single crystals are indispensable for, e.g. measurement of elastic constants of phases by ultrasonic techniques. The neutron diffraction method was used to detect and distinguish the presence of individual lattice correspondence variants of the 2H orthorhombic martensite phase in Cu-Al-Ni as well as to follow the activity of twinning processes during the deformation test on the martensite variant single crystals. When preparing the martensite single variant prism-shaped crystals by compression deformation method, typically a small fraction of second unwanted martensitic variant (compound twin) remains in the prism samples. Due to the very low stress (∼1 MPa) for the compound twinning in many shape memory alloys, it is quite difficult not only to deplete the martensite prisms of all internal interfaces but mainly to keep them in the martensite single variant state for a long time needed for further investigations

  12. Water activated doping and transport in multilayered germanane crystals

    International Nuclear Information System (INIS)

    Young, Justin R; Johnston-Halperin, Ezekiel; Chitara, Basant; Cultrara, Nicholas D; Arguilla, Maxx Q; Jiang, Shishi; Fan, Fan; Goldberger, Joshua E

    2016-01-01

    The synthesis of germanane (GeH) has opened the door for covalently functionalizable 2D materials in electronics. Herein, we demonstrate that GeH can be electronically doped by incorporating stoichiometric equivalents of phosphorus dopant atoms into the CaGe 2 precursor. The electronic properties of these doped materials show significant atmospheric sensitivity, and we observe a reduction in resistance by up to three orders of magnitude when doped samples are measured in water-containing atmospheres. This variation in resistance is a result of water activation of the phosphorus dopants. Transport measurements in different contact geometries show a significant anisotropy between in-plane and out-of-plane resistances, with a much larger out-of-plane resistance. These measurements along with finite element modeling results predict that the current distribution in top-contacted crystals is restricted to only the topmost, water activated crystal layers. Taken together, these results pave the way for future electronic and optoelectronic applications utilizing group IV graphane analogues. (paper)

  13. Structural peculiarities and point defects of bulk-ZnO single crystals

    International Nuclear Information System (INIS)

    Kaurova, I.A.; Kuz’micheva, G.M.; Rybakov, V.B.; Cousson, A.; Gayvoronsky, V.Ya.

    2014-01-01

    Highlights: • ZnO single crystals of different color were grown by the hydrothermal method. • Point defects in ZnO have been firstly investigated by neutron diffraction. • Presence of additional reflections caused by kinetic growth effects was revealed. • The relationship between the color and zinc and oxygen vacancies was found. • Photoinduced variation of transmittance versus the CW laser intensity was analyzed. - Abstract: ZnO single crystals are related to promising direct wide band gap semiconductor materials belonging to the A II B VI type of compounds with wurtzite structure. “Unintentional” n-type conductivity in ZnO may be caused by zinc and oxygen vacancies, and interstitial zinc atoms. To date, the comprehensive structural investigation and analysis of point defects in ZnO is absent in literature. Green, light green and almost colorless ZnO single crystals grown by the hydrothermal method in concentrated alkali solutions 4M(KOH) + 1M(LiOH) + 0.1M(NH 4 OH) on monohedral seeds [0 0 0 1] at crystallization temperatures in the range of 330–350 °C and pressures in the range of 30–50 MPa have been firstly investigated by neutron diffraction. It was revealed the presence of additional reflections (∼12–∼16%) for all the crystals caused by kinetic growth effects that give grounds to assign them to the space group P3 rather than to P6 3 mc. Analysis of the refined compositions together with the color of ZnO crystals does not rule out the relationship between the color and vacancies in the zinc and oxygen positions whose concentration decreases with the discoloration of the samples. The analysis of the photoinduced variation of the total and on-axis transmittance versus the CW laser intensity showed that the colored samples have profound deep defects related to oxygen vacancies

  14. Effects of Photonic Crystals on the Light Output of Heavy Inorganic Scintillators

    CERN Document Server

    Knapitsch, Arno; Fabjan, Christian W; Leclercq, Jean-Louis; Letartre, Xavier; Mazurczyk, Radoslaw; Lecoq, Paul

    2013-01-01

    Photonic crystals (PhCs) are optical materials which can affect the propagation of light in multiple ways. In recent years PhCs contributed to major technological developments in the field of semiconductor lasers, light emitting diodes and photovoltaic applications. In our case we are investigating the capabilities of photonic crystal slabs with the aim to improve the performance of heavy inorganic scintillators. To study the combination of scintillators and PhCs we use a Monte-Carlo program to simulate the light propagation inside a scintillator and a rigorous coupled wave analysis (RCWA) framework to analyse the optical PhC properties. The simulations show light output improvements of a wide range of scintillating materials due to light scattering effects of the PhC slabs. First samples have been produced on top of 1.2 × 2.6 × 5 mm LSO (cerium-doped Lutetium Oxyorthosilicate, Lu_2SiO_5:Ce^3+) scintillators using electron beam lithography and reactive ion etching (RIE). Our samples show a 30-60% light outp...

  15. A systematic study of the isothermal crystallization of the mono-alcohol n-butanol monitored by dielectric spectroscopy

    DEFF Research Database (Denmark)

    Jensen, Mikkel Hartmann; Hecksher, Tina; Niss, Kristine

    2015-01-01

    Isothermal crystallization of the mono-hydroxyl alcohol n-butanol was studied with dielectric spectroscopy in real time. The crystallization was carried out using two different sample cells at 15 temperatures between 120 K and 134 K. Crystallization is characterized by a decrease of the dielectric...... intensity. In addition, a shift in relaxation times to shorter times was observed during the crystallization process for all studied temperatures. The two different sample environments induced quite different crystallization behaviors, consistent and reproducible over all studied temperatures...... that a microscopic interpretation of crystallization measurements requires multiple probes, sample cells, and protocols....

  16. Investigation on structural aspects of ZnO nano-crystal using radio-active ion beam and PAC

    Energy Technology Data Exchange (ETDEWEB)

    Ganguly, Bichitra Nandi, E-mail: bichitra.ganguly@saha.ac.in [Saha Institute of Nuclear Physics, Kolkata 700064 (India); Dutta, Sreetama; Roy, Soma [Saha Institute of Nuclear Physics, Kolkata 700064 (India); Röder, Jens [Physics Department, ISOLDE/CERN, Geneva (Switzerland); Physical Chemistry, RWTH-Aachen, Aachen (Germany); Johnston, Karl [Physics Department, ISOLDE/CERN, Geneva (Switzerland); Experimental Physics, University of the Saarland, Saarbrücken (Germany); Martin, Manfred [Physical Chemistry, RWTH-Aachen, Aachen (Germany)

    2015-11-01

    Nano-crystalline ZnO has been studied with perturbed angular correlation using {sup 111m}Cd, implanted at ISOLDE/CERN and X-ray diffraction using Rietveld analysis. The data show a gradual increase in the crystal size and stress for a sample annealed at 600 °C, and reaching nearly properties of standard ZnO with tempering at 1000 °C. The perturbed angular correlation data show a broad frequency distribution at low annealing temperatures and small particle sizes, whereas at high annealing temperature and larger crystal sizes, results similar to bulk ZnO have been obtained. The ZnO nano-crystalline samples were initially prepared through a wet chemical route, have been examined by Fourier Transform Infrared Spectroscopy (FT-IR) and chemical purity has been confirmed with Energy Dispersive X-ray (EDAX) analysis as well as Transmission Electron Microscopy (TEM).

  17. Automation of High-Throughput Crystal Screening and Data Collection at SSRL

    International Nuclear Information System (INIS)

    Miller, Mitchell D.; Brinen, Linda S.; Deacon, Ashley M.; Bedem, Henry van den; Wolf, Guenter; Xu Qingping; Zhang Zepu; Cohen, Aina; Ellis, Paul; McPhillips, Scott E.; McPhillips, Timothy M.; Phizackerley, R. Paul; Soltis, S. Michael

    2004-01-01

    A robotic system for auto-mounting crystals from liquid nitrogen is now operational on SSRL beamlines (Cohen et al., J. Appl. Cryst. (2002). 35, 720-726). The system uses a small industrial 4-axis robot with a custom built actuator. Once mounted, automated alignment of the sample loop to the X-ray beam readies the crystal for data collection. After data collection, samples are returned to the cassette. The beamline Dewar accommodates three compact sample cassettes (holding up to 96 samples each). During the past 4 months, the system on beamline 11-1 has been used to screen over 1000 crystals. The system has reduced both screening time and manpower. Integration of the hardware components is accomplished in the Distributed Control System architecture developed at SSRL (McPhillips et al., J. Synchrotron Rad. (2002) 9, 401-406). A crystal-screening interface has been implemented in Blu-Ice. Sample details can be uploaded from an Excel spreadsheet. The JCSG generates these spreadsheets automatically from their tracking database using standard database tools (http://www.jcsg.org). New diffraction image analysis tools are being employed to aid in extracting results. Automation also permits tele-presence. For example, samples have been changed during the night without leaving home and scientists have screened crystals 1600 miles from the beamline. The system developed on beamline 11-1 has been replicated onto 1-5, 9-1, 9-2, and 11-3 and is used by both general users and the JCSG

  18. Pinning-to-barrier crossover in YBa2Cu3O7-δ single crystals

    Science.gov (United States)

    Indenbom, M. V.; van der Beek, C. J.; Berseth, V.; Konczykowski, M.; Holtzberg, F.; Benoit, W.

    1996-03-01

    The behaviour of magnetic flux in high purity untwinned YBa2Cu3O7-δ (YBCO) single crystals is visualised by means of the magneto-optical technique. It is observed that after zero field-cooling at high temperatures near T c , flux penetrates directly to the sample center over a flux free edge area, in contrast to the usual Bean-like flux penetration from the edges. This fact clearly shows that volume pinning becomes negligible compared with the edge barrier. The role of the recently rediscovered geometrical barrier in the crystal magnetisation is discussed.

  19. The crystallization of (NiCu)ZrTiAlSi glass/crystalline composite

    International Nuclear Information System (INIS)

    Czeppe, T.; Sypien, A.; Ochin, P.; Anastassova, S.

    2007-01-01

    Alloys of composition (Ni 1-x Cu x ) 60 Zr 18 Ti 13 A1 5 Si 4 were investigated in the form of ribbons and massive samples. The microstructure of the massive samples consists of dendritic crystals in the amorphous or nanocrystalline matrix. The amount of the amorphous phase is the lowest in the sample with the highest Cu content. The segregation in the liquid phase, leading to the local differences in density and the composition of the crystallizing dendrites in the samples crystallized in the copper mould was shown. The typical compositions of the multi-component crystals could be distinguished; one with the increased content of aluminum, the second with the high content of silicon and third, with the high content of (NiCu) and (ZrTi). The cubic phase Ni(Cu)Ti(Zr) with Cu and Zr dissolved could be identified. (Abstract Copyright [2007], Wiley Periodicals, Inc.)

  20. 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.

  1. Induced defects in neutron irradiated GaN single crystals

    International Nuclear Information System (INIS)

    Park, I. W.; Koh, E. K.; Kim, Y. M.; Choh, S. H.; Park, S. S.; Kim, B. G.; Sohn, J. M.

    2005-01-01

    The local structure of defects in undoped, Si-doped, and neutron irradiated free standing GaN bulk crystals, grown by hydride vapor phase epitaxy, has been investigated by employing Raman scattering and cathodoluminescence. The GaN samples were irradiated to a dose of 2 x 10 17 neutrons in an atomic reactor at Korea Atomic Energy Research Institute. There was no appreciable change in the Raman spectra for undoped GaN samples before and after neutron irradiation. However, a forbidden transition, A 1 (TO) mode, appeared for a neutron irradiated Si-doped GaN crystal. Cathodoluminescence spectrum for the neutron irradiated Si-doped GaN crystal became much more broadened than that for the unirradiated one. The experimental results reveal the generation of defects with locally deformed structure in the wurtzite Si-doped GaN single crystal

  2. Synthesis and characterization of p-type boron-doped IIb diamond large single crystals

    International Nuclear Information System (INIS)

    Li Shang-Sheng; Li Xiao-Lei; Su Tai-Chao; Jia Xiao-Peng; Ma Hong-An; Huang Guo-Feng; Li Yong

    2011-01-01

    High-quality p-type boron-doped IIb diamond large single crystals are successfully synthesized by the temperature gradient method in a china-type cubic anvil high-pressure apparatus at about 5.5 GPa and 1600 K. The morphologies and surface textures of the synthetic diamond crystals with different boron additive quantities are characterized by using an optical microscope and a scanning electron microscope respectively. The impurities of nitrogen and boron in diamonds are detected by micro Fourier transform infrared technique. The electrical properties including resistivities, Hall coefficients, Hall mobilities and carrier densities of the synthesized samples are measured by a four-point probe and the Hall effect method. The results show that large p-type boron-doped diamond single crystals with few nitrogen impurities have been synthesized. With the increase of quantity of additive boron, some high-index crystal faces such as {113} gradually disappear, and some stripes and triangle pits occur on the crystal surface. This work is helpful for the further research and application of boron-doped semiconductor diamond. (cross-disciplinary physics and related areas of science and technology)

  3. Pressure-induced effects on the spectroscopic properties of Nd{sup 3+} in MgO:LiNbO{sub 3} single crystal. A crystal field approach

    Energy Technology Data Exchange (ETDEWEB)

    Muñoz Santiuste, J.E., E-mail: jems@fis.uc3m.es [Departamento de Física, Escuela Politécnica Superior, Universidad Carlos III de Madrid, Avenida de la Universidad 30, E-28913 Leganés, Madrid (Spain); MALTA Consolider Team (Spain); Lavín, V.; Rodríguez-Mendoza, U.R. [MALTA Consolider Team (Spain); Departamento de Física, INM and IUdEA, Universidad de La Laguna, Apdo. 456. E-38200 San Cristóbal de La Laguna, Santa Cruz de Tenerife (Spain); Tardio, M.M.; Ramírez-Jiménez, R. [Departamento de Física, Escuela Politécnica Superior, Universidad Carlos III de Madrid, Avenida de la Universidad 30, E-28913 Leganés, Madrid (Spain)

    2017-04-15

    The effects of pressure on the Nd{sup 3+}-doped MgO:LiNbO{sub 3} single crystal have been studied by luminescence spectroscopy at low temperature and high pressures from ambient conditions up to 33 GPa. Specifically, the pressure-induced evolution of the emission spectra, corresponding to the {sup 4}F{sub 3/2}→{sup 4}I{sub 9/2},{sup 4}I{sub 11/2} transitions, and the excitation spectra, corresponding to the {sup 4}I{sub 9/2}→{sup 4}F{sub 5/2}+{sup 2}H{sub 9/2}, and {sup 4}I{sub 9/2}→{sup 4}F{sub 7/2}+{sup 4}S{sub 3/2} transitions, show a gradual red-shift that follows a linear pressure dependence and a decrease in the intensity of the spectra with increasing pressure. The initial effect of increasing pressure on the MgO:LiNbO{sub 3} crystal is the modification of the relative amount of the several centers in the sample. At pressures around 20 GPa the characteristic multicenter Nd{sup 3+} structure eventually disappears indicating that all the centers have very similar environments near this pressure. At higher pressures, observed changes seem to have a different origin. The evolution of Nd{sup 3+} luminescence is studied in the frame of crystal-field theory in order to evaluate its capability of monitoring the pressure-induced structural changes. Crystal-field analysis, under approximated C{sub 3v} symmetry, shows a smooth increase of the overall crystal-field strength on the luminescent ion, which can be related to the volume reduction as pressure increases. Crystal-field parameters also show a general monotonic behavior with pressure that indicates a structural modification of the local structure that, maintaining the trigonal symmetry around the impurity ion, evolves towards a lower axial character. No evidences of a phase transition have been observed in the studied pressure range.

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

    Science.gov (United States)

    2017-10-09

    for AGG should be minimal. For this purpose, the seeds for AGG may also be provided externally. This process is called the solid-state single...bonding process . Figure 31 shows (a) the growth of one large single crystal from one small single crystal seed as well as (b) the growth of one...one bi-crystal seed : One large bi-crystal can be grown from one small bi-crystal by SSCG process . Fig. 32. Diffusion bonding process for

  5. The role of crystal orientation and surface proximity in the self-similar behavior of deformed Cu single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Pang, Judy W.L., E-mail: pangj@ornl.gov [Materials Science and Technology Division, Oak Ridge National Laboratory, 1 Behtel Valley Road, Oak Ridge, TN 37831 (United States); Ice, Gene E. [Materials Science and Technology Division, Oak Ridge National Laboratory, 1 Behtel Valley Road, Oak Ridge, TN 37831 (United States); Liu Wenjun [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States)

    2010-11-25

    We report on novel 3D spatially resolved X-ray diffraction microscopy studies of self-affine behavior in deformed single crystals. This study extends surface profile measurements of self-affined morphology changes in single crystals during deformation to include local lattice rotations and sub-surface behavior. Investigations were made on the spatial correlation of the local lattice rotations in 8% tensile deformed Cu single crystals oriented with [1 2 3], [1 1 1] and [0 0 1] axes parallel to the tensile axis. The nondestructive depth-resolved measurements were made over a length scale of one to hundreds of micrometers. Self-affined correlation was found both at the surface and below the surface of the samples. A universal exponent for the power-law similar to that observed with surface profile methods is found at the surface of all samples but crystallographically sensitive changes are observed as a function of depth. Correlation lengths of the self-affine behavior vary with the [1 2 3] crystal exhibiting the longest self-affine length scale of 70 {mu}m with only 18 {mu}m for the [1 1 1] and [0 0 1] crystals. These measurements illuminate the transition from surface-like to bulk-like deformation behavior and provide new quantitative information to guide emerging models of self-organized structures in plasticity.

  6. Pyroelectric Study on Dipolar Alignment in 0.69Pb(Mg1/3Nb2/3)O3-0.31PbTiO3 Single Crystals

    Institute of Scientific and Technical Information of China (English)

    ZHAO Liang; SHEN Ming-Rong; CAO Wen-Wu

    2012-01-01

    Pyroelectric measurements are conducted during zero-Geld heating in [001], [110] and [111] poled 0.69Pb(Mg1/3 Nb2/3)O3-0.31PbTiO3 single crystals. Compared to the room-temperature-poled samples, the crystals poled by using the Rield cooling method show broad but well recognizable pyroelectric current peaks near 190℃, which is much higher than the Curie point (126℃) of the crystal. We propose that this peak of the crystals poled by field-cooling above the Curie point is ascribed to the order-disorder transition of the dipoles in polar nano-regions formed at the Burns temperature.%Pyroelectric measurements are conducted during zero-field heating in [001],[110] and [111] poled 0.69Pb(Mg1/3Nb2/3)O3-0.31PbTiO3 single crystals.Compared to the room-temperature-poled samples,the crystals poled by using the field cooling method show broad but well recognizable pyroelectric current peaks near 190℃,which is much higher than the Curie point (126℃) of the crystal.We propose that this peak of the crystals poled by field-cooling above the Curie point is ascribed to the order-disorder transition of the dipoles in polar nano-regions formed at the Burns temperature.

  7. Desorption of Water from Distinct Step Types on a Curved Silver Crystal

    Directory of Open Access Journals (Sweden)

    Jakrapan Janlamool

    2014-07-01

    Full Text Available We have investigated the adsorption of H2O onto the A and B type steps on an Ag single crystal by temperature programmed desorption. For this study, we have used a curved crystal exposing a continuous range of surface structures ranging from [5(111 × (100] via (111 to [5(111 × (110]. LEED and STM studies verify that the curvature of our sample results predominantly from monoatomic steps. The sample thus provides a continuous array of step densities for both step types. Desorption probed by spatially-resolved TPD of multilayers of H2O shows no dependence on the exact substrate structure and thus confirms the absence of thermal gradients during temperature ramps. In the submonolayer regime, we observe a small and linear dependence of the desorption temperature on the A and B step density. We argue that such small differences are only observable by means of a single curved crystal, which thus establishes new experimental benchmarks for theoretical calculation of chemically accurate binding energies. We propose an origin of the observed behavior based on a “two state” desorption model.

  8. The plug-based nanovolume Microcapillary Protein Crystallization System (MPCS)

    International Nuclear Information System (INIS)

    Gerdts, Cory J.; Elliott, Mark; Lovell, Scott; Mixon, Mark B.; Napuli, Alberto J.; Staker, Bart L.; Nollert, Peter; Stewart, Lance

    2008-01-01

    The Microcapillary Protein Crystallization System (MPCS) is a new protein-crystallization technology used to generate nanolitre-sized crystallization experiments for crystal screening and optimization. Using the MPCS, diffraction-ready crystals were grown in the plastic MPCS CrystalCard and were used to solve the structure of methionine-R-sulfoxide reductase. The Microcapillary Protein Crystallization System (MPCS) embodies a new semi-automated plug-based crystallization technology which enables nanolitre-volume screening of crystallization conditions in a plasticware format that allows crystals to be easily removed for traditional cryoprotection and X-ray diffraction data collection. Protein crystals grown in these plastic devices can be directly subjected to in situ X-ray diffraction studies. The MPCS integrates the formulation of crystallization cocktails with the preparation of the crystallization experiments. Within microfluidic Teflon tubing or the microfluidic circuitry of a plastic CrystalCard, ∼10–20 nl volume droplets are generated, each representing a microbatch-style crystallization experiment with a different chemical composition. The entire protein sample is utilized in crystallization experiments. Sparse-matrix screening and chemical gradient screening can be combined in one comprehensive ‘hybrid’ crystallization trial. The technology lends itself well to optimization by high-granularity gradient screening using optimization reagents such as precipitation agents, ligands or cryoprotectants

  9. Growth and surface topography of WSe_2 single crystal

    International Nuclear Information System (INIS)

    Dixit, Vijay; Vyas, Chirag; Pataniya, Pratik; Jani, Mihir; Pathak, Vishal; Patel, Abhishek; Pathak, V. M.; Patel, K. D.; Solanki, G. K.

    2016-01-01

    Tungsten Di-Selenide belongs to the family of TMDCs showing their potential applications in the fields of Optoelectronics and PEC solar cells. Here in the present investigation single crystals of WSe_2 were grown by Direct Vapour Transport Technique in a dual zone furnace having temperature difference of 50 K between the two zones. These single crystals were characterized by EDAX which confirms the stiochiometry of the grown crystals. Surface topography of the crystal was studied by optical micrograph showing the left handed spirals on the surface of WSe_2 crystals. Single crystalline nature of the crystals was confirmed by SAED.

  10. Structure in a confined smectic liquid crystal with competing surface and sample elasticities

    International Nuclear Information System (INIS)

    Idziak, S.H.; Koltover, I.; Israelachvili, J.N.; Safinya, C.R.

    1996-01-01

    We report on studies using the x-ray surface forces apparatus (XSFA) to compare the structure of a liquid crystal confined between hard surfaces and, for the first time, between soft surfaces that can deform due to the stresses imposed by the confined fluid. We find that the alignment of smectic domains in confined films depends critically on both the shape and compliance of the confining walls or surfaces: open-quote open-quote Soft surfaces close-quote close-quote exhibit a critical gap thickness of 3.4 μm for the liquid crystal studied at which maximum alignment occurs, while open-quote open-quote hard surfaces close-quote close-quote do not exhibit gap-dependent alignment. copyright 1996 The American Physical Society

  11. Transport properties of PrxOs4Sb12 single crystals with high Pr-site filling fraction grown under high pressure

    International Nuclear Information System (INIS)

    Tanaka, Kenya; Namiki, Takahiro; Saito, Takashi; Tatsuoka, Sho; Imamura, Atsushi; Kuwahara, Keitaro; Aoki, Yuji; Sato, Hideyuki

    2009-01-01

    We have succeeded in growing Pr x Os 4 Sb 12 single crystals under ∼4GPa with high Pr-site filling fraction x. The electrical resistance measurements clearly show that the superconducting (SC) transition is sharper and the onset temperatures is lower in the single crystal samples grown under high pressure compared to that of the sample grown under ambient pressure. These results suggest that the double SC transition ascribed to sample inhomogeneity is suppressed in the sample grown under high pressure. The change of 4f-electron crystalline electric field energy splitting between the Γ 1 ground state and the Γ 4 (2) first excited state in the sample made under high pressure is proposed as one of the possible origins of the suppression of the double SC transition.

  12. Crystal-chemical characteristics of nontronites from bottom sediments of Pacific ocean

    International Nuclear Information System (INIS)

    Palchik, N. A.; Moroz, T. N.; Grigorieva, T. N.; Nikandrova, N. K.; Miroshnichenko, L. V.

    2017-01-01

    A crystal-chemical analysis of the nontronite samples formed in deep-water sediments of the underwater Juan-de-Fuca ridge in the Pacific ocean has been performed using powder X-ray diffraction, IR spectroscopy, and Mössbauer spectroscopy. A comparison with the previously investigated nontronites from different regions of the Sea of Okhotsk showed that the structural features of these formations are due to the difference in the physicochemical parameters of their crystallization. The values of the basal interplanar spacing d_0_0_1 (within 11–13 Å) in the samples analyzed are determined by the degree of hydration and cation filling of the interlayer space, while the differences in the IR spectra are due to isomorphic substitutions in the structure. The character of cation distribution and the nature and concentration of stacking faults in nontronite structures are determined. The differences in the composition, structure, and properties of nontronites of different origin are confirmed by theoretical calculations of their structural parameters.

  13. Crystal-chemical characteristics of nontronites from bottom sediments of Pacific ocean

    Energy Technology Data Exchange (ETDEWEB)

    Palchik, N. A., E-mail: nadezhda@igm.nsc.ru; Moroz, T. N.; Grigorieva, T. N. [Russian Academy of Sciences, Sobolev Institute of Geology and Mineralogy, Siberian Branch (Russian Federation); Nikandrova, N. K. [Russian Academy of Sciences, Institute of Mineralogy, Ural Branch (Russian Federation); Miroshnichenko, L. V. [Russian Academy of Sciences, Sobolev Institute of Geology and Mineralogy, Siberian Branch (Russian Federation)

    2017-01-15

    A crystal-chemical analysis of the nontronite samples formed in deep-water sediments of the underwater Juan-de-Fuca ridge in the Pacific ocean has been performed using powder X-ray diffraction, IR spectroscopy, and Mössbauer spectroscopy. A comparison with the previously investigated nontronites from different regions of the Sea of Okhotsk showed that the structural features of these formations are due to the difference in the physicochemical parameters of their crystallization. The values of the basal interplanar spacing d{sub 001} (within 11–13 Å) in the samples analyzed are determined by the degree of hydration and cation filling of the interlayer space, while the differences in the IR spectra are due to isomorphic substitutions in the structure. The character of cation distribution and the nature and concentration of stacking faults in nontronite structures are determined. The differences in the composition, structure, and properties of nontronites of different origin are confirmed by theoretical calculations of their structural parameters.

  14. 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.

  15. 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.

  16. Evaluation of the physical stability and local crystallization of amorphous terfenadine using XRD-DSC and micro-TA

    International Nuclear Information System (INIS)

    Yonemochi, Etsuo; Hoshino, Takafumi; Yoshihashi, Yasuo; Terada, Katsuhide

    2005-01-01

    It is very difficult to follow rapid changes in polymorphic transformation and crystallization and to estimate the species recrystallized from the amorphous form. The aim of this study was to clarify the structural changes of amorphous terfenadine and to evaluate the polymorphs crystallized from amorphous samples using XRD-DSC and an atomic force microscope with a thermal probe (micro-TA). Amorphous samples were prepared by grinding or rapid cooling of the melt. The rapid structural transitions of samples were followed by the XRD-DSC system. On the DSC trace of the quenched terfenadine, two exotherms were observed, while only one exothermic peak was observed in the DSC scan of a ground sample. From the in situ data obtained by the XRD-DSC system, the stable form of terfenadine was recrystallized during heating of the ground amorphous sample, whereas the metastable form was recrystallized from the quenched amorphous sample and the crystallized polymorph changed to the stable form. Obtained data suggested that recrystallized species could be related to the homogeneity of samples. When the stored sample surface was scanned by atomic force microscopy (AFM), heterogeneous crystallization was observed. By using micro-TA, melting temperatures at various points were measured, and polymorph forms I and II were crystallized in each region. The percentages of the crystallized form I stored at 120 and 135 deg C were 47 and 79%, respectively. This result suggested that increasing the storage temperature increased the crystallization of form I, the stable form, confirming the temperature dependency of the crystallized form. The crystallization behavior of amorphous drug was affected by the annealing temperature. Micro-TA would be useful for detecting the inhomogeneities in polymorphs crystallized from amorphous drug

  17. Pressures of Partial Crystallization of Magmas Along Transforms: Implications for Crustal Accretion

    Science.gov (United States)

    Scott, J. L.; Zerda, C.; Brown, D.; Ciaramitaro, S. C.; Barton, M.

    2016-12-01

    Plate spreading at mid-ocean ridges is responsible for the creation of most of the crust on earth. The ridge system is very complex and many questions remain unresolved. Among these is the nature of magma plumbing systems beneath transform faults. Pervious workers have suggested that increased conductive cooling along transforms promotes higher pressures of partial crystallization, and that this explains the higher partial pressures of crystallization inferred for magmas erupted along slow spreading ridges compared to magmas erupted along faster spreading ridges. To test this hypothesis, we undertook a detailed analysis of pressures of partial crystallization for magmas erupted at 3 transforms along the fast to intermediate spreading East Pacific Rise(Blanco, Clipperton, and Siqueiros) and 3 transforms along the slow spreading Mid Atlantic Ridge(Famous Transform B, Kane, and 15°20'N). Pressures of partial crystallization were calculated from the compositions of glasses (quenched liquids) lying along the P (and T) dependent olivine, plagioclase, and augite cotectic using the method described by Kelley and Barton (2008). Published analyses of mid-ocean ridge basalt glasses sampled from these transforms and surrounding ridge segments were used as input data. Samples with anomalous chemical compositions and samples that yielded pressures associated with unrealistically large uncertainties were filtered out of the database. The pressures of partial crystallization for the remaining 916 samples ranged from 0 to 520 MPa with the great majority ( 95%) of sample returning pressures of less than 300 MPa. Pressures of 300 MPa) are associated with a small number of samples from the Pacific segments. Except for the Blanco, pressures of partial crystallization do not increase as transforms are approached. These observations contrast with those of previous workers, who reported anomalously high pressures (up to 1000 MPa) for a large number of samples erupted near both Atlantic

  18. Investigation of lactose crystallization process during condensed milk cooling using native vacuum-crystallizer

    Directory of Open Access Journals (Sweden)

    E. I. Dobriyan

    2016-01-01

    Full Text Available One of the most general defects of condensed milk with sugar is its consistency heterogeneity – “candying”. The mentioned defect is conditioned by the presence of lactose big crystals in the product. Lactose crystals size up to 10 µm is not organoleptically felt. The bigger crystals impart heterogeneity to the consistency which can be evaluated as “floury”, “sandy”, “crunch on tooth”. Big crystals form crystalline deposit on the can or industrial package bottom in the form of thick layer. Industrial processing of the product with the defective process of crystallization results in the expensive equipment damage of the equipment at the confectionary plant accompanied with heavy losses. One of the factors influencing significantly lactose crystallization is the product cooling rate. Vacuum cooling is the necessary condition for provision of the product consistency homogeneity. For this purpose the vacuum crystallizers of “Vigand” company, Germany, are used. But their production in the last years has been stopped. All-Russian dairy research institute has developed “The references for development of the native vacuum crystallizer” according to which the industrial model has been manufactured. The produced vacuum – crystallizer test on the line for condensed milk with sugar production showed that the product cooling on the native vacuum-crystallizer guarantees production of the finished product with microstructure meeting the requirements of State standard 53436–2009 “Canned Milk. Milk and condensed cream with sugar”. The carried out investigations evidences that the average lactose crystals size in the condensed milk with sugar cooled at the native crystallizer makes up 6,78 µm. The granulometric composition of the product crystalline phase cooled at the newly developed vacuum-crystallizer is completely identical to granulometric composition of the product cooled at “Vigand” vacuum-crystallizer.

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

    Science.gov (United States)

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

    2018-04-01

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

  20. Tailoring of silicon crystals for relativistic-particle channeling

    International Nuclear Information System (INIS)

    Guidi, V.; Antonini, A.; Baricordi, S.; Logallo, F.; Malagu, C.; Milan, E.; Ronzoni, A.; Stefancich, M.; Martinelli, G.; Vomiero, A.

    2005-01-01

    In the last years, the research on channeling of relativistic particles has progressed considerably. A significant contribution has been provided by the development of techniques for quality improvement of the crystals. In particular, a planar etching of the surfaces of the silicon crystals proved useful to remove the superficial layer, which is a region very rich in imperfections, in turn leading to greater channeling efficiency. Micro-fabrication techniques, borrowed from silicon technology, may also be useful: micro-indentation and deposition of tensile or compressive layers onto silicon samples allow one to impart an even curvature to the samples. In this way, different topologies may be envisaged, such as a bent crystal for deflection of protons and ions or an undulator to force coherent oscillations of positrons and electrons

  1. Fully automatic characterization and data collection from crystals of biological macromolecules

    International Nuclear Information System (INIS)

    Svensson, Olof; Malbet-Monaco, Stéphanie; Popov, Alexander; Nurizzo, Didier; Bowler, Matthew W.

    2015-01-01

    A fully automatic system has been developed that performs X-ray centring and characterization of, and data collection from, large numbers of cryocooled crystals without human intervention. Considerable effort is dedicated to evaluating macromolecular crystals at synchrotron sources, even for well established and robust systems. Much of this work is repetitive, and the time spent could be better invested in the interpretation of the results. In order to decrease the need for manual intervention in the most repetitive steps of structural biology projects, initial screening and data collection, a fully automatic system has been developed to mount, locate, centre to the optimal diffraction volume, characterize and, if possible, collect data from multiple cryocooled crystals. Using the capabilities of pixel-array detectors, the system is as fast as a human operator, taking an average of 6 min per sample depending on the sample size and the level of characterization required. Using a fast X-ray-based routine, samples are located and centred systematically at the position of highest diffraction signal and important parameters for sample characterization, such as flux, beam size and crystal volume, are automatically taken into account, ensuring the calculation of optimal data-collection strategies. The system is now in operation at the new ESRF beamline MASSIF-1 and has been used by both industrial and academic users for many different sample types, including crystals of less than 20 µm in the smallest dimension. To date, over 8000 samples have been evaluated on MASSIF-1 without any human intervention

  2. Fully automatic characterization and data collection from crystals of biological macromolecules

    Energy Technology Data Exchange (ETDEWEB)

    Svensson, Olof; Malbet-Monaco, Stéphanie; Popov, Alexander; Nurizzo, Didier, E-mail: nurizzo@esrf.fr [European Synchrotron Radiation Facility, 71 Avenue des Martyrs, CS 40220, 38043 Grenoble (France); Bowler, Matthew W., E-mail: nurizzo@esrf.fr [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); European Synchrotron Radiation Facility, 71 Avenue des Martyrs, CS 40220, 38043 Grenoble (France)

    2015-07-31

    A fully automatic system has been developed that performs X-ray centring and characterization of, and data collection from, large numbers of cryocooled crystals without human intervention. Considerable effort is dedicated to evaluating macromolecular crystals at synchrotron sources, even for well established and robust systems. Much of this work is repetitive, and the time spent could be better invested in the interpretation of the results. In order to decrease the need for manual intervention in the most repetitive steps of structural biology projects, initial screening and data collection, a fully automatic system has been developed to mount, locate, centre to the optimal diffraction volume, characterize and, if possible, collect data from multiple cryocooled crystals. Using the capabilities of pixel-array detectors, the system is as fast as a human operator, taking an average of 6 min per sample depending on the sample size and the level of characterization required. Using a fast X-ray-based routine, samples are located and centred systematically at the position of highest diffraction signal and important parameters for sample characterization, such as flux, beam size and crystal volume, are automatically taken into account, ensuring the calculation of optimal data-collection strategies. The system is now in operation at the new ESRF beamline MASSIF-1 and has been used by both industrial and academic users for many different sample types, including crystals of less than 20 µm in the smallest dimension. To date, over 8000 samples have been evaluated on MASSIF-1 without any human intervention.

  3. Microstructural, optical and electrical properties of Cl-doped CdTe single crystals

    Directory of Open Access Journals (Sweden)

    Choi Hyojeong

    2016-09-01

    Full Text Available Microstructural, optical and electrical properties of Cl-doped CdTe crystals grown by the low pressure Bridgman (LPB method were investigated for four different doping concentrations (unintentionally doped, 4.97 × 1019 cm−3, 9.94 × 1019 cm−3 and 1.99 × 1020 cm−3 and three different locations within the ingots (namely, samples from top, middle and bottom positions in the order of the distance from the tip of the ingot. It was shown that Cl dopant suppressed the unwanted secondary (5 1 1 crystalline orientation. Also, the average size and surface coverage of Te inclusions decreased with an increase in Cl doping concentration. Spectroscopic ellipsometry measurements showed that the optical quality of the Cl-doped CdTe single crystals was enhanced. The resistivity of the CdTe sample doped with Cl at the 1.99 × 1020 cm−3 was above 1010 Ω.cm.

  4. Crystal growth and mechanical hardness of In{sub 2}Se{sub 2.7}Sb{sub 0.3} single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Patel, Piyush, E-mail: piyush-patel130@yahoo.com; Vyas, S. M., E-mail: s-m-vyas-gu@hotmail.com; Patel, Vimal; Pavagadhi, Himanshu [Department of Physics, School of Science, Gujarat University, Ahmedabad, Gujarat, India-380009 (India); Solanki, Mitesh [panditdindayal Petroleum University, Gandhinagar. Gujarat (India); Jani, Maunik P. [BITS Edu Campus, Varnama, Vadodara, Gujarat (India)

    2015-08-28

    The III-VI compound semiconductors is important for the fabrication of ionizing radiation detectors, solid-state electrodes, and photosensitive heterostructures, solar cell and ionic batteries. In this paper, In{sub 2}Se{sub 2.7} Sb{sub 0.3} single crystals were grown by the Bridgman method with temperature gradient of 60 °C/cm and the growth velocity 0.5cm/hr. The as-grown crystals were examined under the optical microscope for surface study, a various growth features observed on top free surface of the single crystal which is predominant of layers growth mechanism. The lattice parameters of as-grown crystal was determined by the XRD analysis. A Vickers’ projection microscope were used for the study of microhardness on the as-cleaved, cold-worked and annealed samples of the crystals, the results were discussed, and reported in detail.

  5. Light assisted drying (LAD) for protein stabilization: optical characterization of samples

    Science.gov (United States)

    Young, Madison A.; McKinnon, Madison E.; Elliott, Gloria D.; Trammell, Susan R.

    2018-02-01

    Light-Assisted Drying (LAD) is a novel biopreservation technique which allows proteins to be immobilized in a dry, amorphous solid at room temperature. Indicator proteins are used in a variety of diagnostic assays ranging from highthroughput 96-well plates to new microfluidic devices. A challenge in the development of protein-based assays is preserving the structure of the protein during production and storage of the assay, as the structure of the protein is responsible for its functional activity. Freeze-drying or freezing are currently the standard for the preservation of proteins, but these methods are expensive and can be challenging in some environments due to a lack of available infrastructure. An inexpensive, simple processing method that enables supra-zero temperature storage of proteins used in assays is needed. Light-assisted drying offers a relatively inexpensive method for drying samples. Proteins suspended in a trehalose solution are dehydrated using near-infrared laser light. The laser radiation speeds drying and as water is removed the sugar forms a protective matrix. The goal of this study is optically characterize samples processed with LAD. We use polarized light imaging (PLI) to look at crystallization kinetics of samples and determine optimal humidity. PLI shows a 62.5% chance of crystallization during LAD processing and negligible crystallization during low RH storage.

  6. Radiation hardness of undoped BGO crystals

    International Nuclear Information System (INIS)

    Sahu, S.K.; Peng, K.C.; Huang, H.C.; Wang, C.H.; Chang, Y.H.; Hou, W.S.; Ueno, K.; Chou, F.I.; Wei, Y.Y.

    1997-01-01

    We measured the radiation hardness of undoped BGO crystals from two different manufacturers. Such crystals are proposed to be used in a small-angle calorimeter of the BELLE detector of the KEK B-factory. Transparency and scintillation light output of the crystals were monitored to see the effect of radiation damage. The crystals show considerable radiation hardness up to 10.2 Mrad equivalent dose, which is much higher than the maximum expected dosage of 500 krad per year of running at BELLE. (orig.)

  7. Ultrastructural studies of synthetic apatite crystals.

    Science.gov (United States)

    Arends, J; Jongebloed, W L

    1979-03-01

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

  8. Lunar Magma Ocean Crystallization: Constraints from Fractional Crystallization Experiments

    Science.gov (United States)

    Rapp, J. F.; Draper, D. S.

    2015-01-01

    The currently accepted paradigm of lunar formation is that of accretion from the ejecta of a giant impact, followed by crystallization of a global scale magma ocean. This model accounts for the formation of the anorthosite highlands crust, which is globally distributed and old, and the formation of the younger mare basalts which are derived from a source region that has experienced plagioclase extraction. Several attempts at modelling the crystallization of such a lunar magma ocean (LMO) have been made, but our ever-increasing knowledge of the lunar samples and surface have raised as many questions as these models have answered. Geodynamic models of lunar accretion suggest that shortly following accretion the bulk of the lunar mass was hot, likely at least above the solidus]. Models of LMO crystallization that assume a deep magma ocean are therefore geodynamically favorable, but they have been difficult to reconcile with a thick plagioclase-rich crust. A refractory element enriched bulk composition, a shallow magma ocean, or a combination of the two have been suggested as a way to produce enough plagioclase to account for the assumed thickness of the crust. Recently however, geophysical data from the GRAIL mission have indicated that the lunar anorthositic crust is not as thick as was initially estimated, which allows for both a deeper magma ocean and a bulk composition more similar to the terrestrial upper mantle. We report on experimental simulations of the fractional crystallization of a deep (approximately 100km) LMO with a terrestrial upper mantle-like (LPUM) bulk composition. Our experimental results will help to define the composition of the lunar crust and mantle cumulates, and allow us to consider important questions such as source regions of the mare basalts and Mg-suite, the role of mantle overturn after magma ocean crystallization and the nature of KREEP

  9. A phoswich detector design for improved spatial sampling in PET

    Science.gov (United States)

    Thiessen, Jonathan D.; Koschan, Merry A.; Melcher, Charles L.; Meng, Fang; Schellenberg, Graham; Goertzen, Andrew L.

    2018-02-01

    Block detector designs, utilizing a pixelated scintillator array coupled to a photosensor array in a light-sharing design, are commonly used for positron emission tomography (PET) imaging applications. In practice, the spatial sampling of these designs is limited by the crystal pitch, which must be large enough for individual crystals to be resolved in the detector flood image. Replacing the conventional 2D scintillator array with an array of phoswich elements, each consisting of an optically coupled side-by-side scintillator pair, may improve spatial sampling in one direction of the array without requiring resolving smaller crystal elements. To test the feasibility of this design, a 4 × 4 phoswich array was constructed, with each phoswich element consisting of two optically coupled, 3 . 17 × 1 . 58 × 10mm3 LSO crystals co-doped with cerium and calcium. The amount of calcium doping was varied to create a 'fast' LSO crystal with decay time of 32.9 ns and a 'slow' LSO crystal with decay time of 41.2 ns. Using a Hamamatsu R8900U-00-C12 position-sensitive photomultiplier tube (PS-PMT) and a CAEN V1720 250 MS/s waveform digitizer, we were able to show effective discrimination of the fast and slow LSO crystals in the phoswich array. Although a side-by-side phoswich array is feasible, reflections at the crystal boundary due to a mismatch between the refractive index of the optical adhesive (n = 1 . 5) and LSO (n = 1 . 82) caused it to behave optically as an 8 × 4 array rather than a 4 × 4 array. Direct coupling of each phoswich element to individual photodetector elements may be necessary with the current phoswich array design. Alternatively, in order to implement this phoswich design with a conventional light sharing PET block detector, a high refractive index optical adhesive is necessary to closely match the refractive index of LSO.

  10. Investigation of crystal structure, dielectric and magnetic properties in La and Nd co-doped BiFeO{sub 3} multiferroics

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Ompal [Department of Physics, Guru Jambheshwar University of Science & Technology, Hisar 125001, Haryana (India); Agarwal, Ashish, E-mail: aagju@yahoo.com [Department of Physics, Guru Jambheshwar University of Science & Technology, Hisar 125001, Haryana (India); Sanghi, Sujata [Department of Physics, Guru Jambheshwar University of Science & Technology, Hisar 125001, Haryana (India); Das, Amitabh [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Anju [Department of Physics, Chaudhary Devi Lal University, Sirsa 125025, Haryana (India)

    2017-03-15

    For the investigation of the crystal structure, dielectric properties and magnetic properties of La and Nd co-doped BiFeO{sub 3} multiferroics; Bi{sub 0.8}La{sub 0.2−x}Nd{sub x}FeO{sub 3} (x=0.075, 0.1, 0.125) samples were prepared through solid state reaction method. Rietveld refinement of the obtained XRD patterns shows that there is change in crystal structure in these samples. At higher concentration of La (at x=0.075), the crystal structure was found to have mixed symmetry with rhombohedral and triclinic phases, while with equal concentration of both the dopants (at x=0.1), the structure changes to mixed symmetry having rhombohedral and orthorhombic phases. At higher concentration of Nd (at x=0.125), again mixed symmetry was established having both phases of the previous composition but approximately in reverse fraction. In dielectric analysis, x=0.1 sample showed the highest values of dielectric constant (ε′) and dielectric loss (tan δ). For x=0.125 sample, it was observed that the dielectric constant and dielectric loss response are improved. The magnetic characterization (M–H loops) indicates the significant enhancement in magnetisation with increasing concentration of Nd. Nd doping leads to the destruction of spiral modulation, forming the antiferromagnets, and visualisation of improved magnetisation via canting of spins. - Highlights: • La and Nd co-doped BiFeO{sub 3} were synthesized. • Change in crystal structure is observed. • Significant enhancement in magnetisation is observed.

  11. LITERATURE SURVEY FOR FRACTIONAL CRYSTALLIZATION STUDY

    International Nuclear Information System (INIS)

    PERSON, J.C.

    2004-01-01

    strain of the crystal. Both the crystal size and the strain in the crystal lattice have a pronounced effect on the growth rate of the individual crystals (Menon 2003). This report is organized into six sections. Section 1 summarizes reports on the design principles for separations by crystallization. Section 2 discusses the fractional crystallization in the NaNO 3 -CH 3 COONa-H 2 O system presented in RPP-18541, ''Test Plan for Tank 241-S-112 Fractional crystallization Study,'' dated 2003. Section 3 summarizes reports on crystallization in the Na 2 CO 3 -Na 2 SO 4 -H 2 O system, which includes the effects of the burkeite double salt (Na 2 CO 3 · 2Na 2 SO 4 ). Section 4 summarizes solubility data for sodium compounds and presents two miscellaneous topics. Section 5 is excerpted from the internet to show applications of thermodynamic calculations. Section 5.1 compares results and calculations for the NaNO 3 -Na 2 SO 4 -H 2 O system, and Section 5.2 shows the use of the calculations to optimize flowsheets. Flowsheets are given for two examples: (1) the production of KNO 3 from NaNO 3 and KCl (including the effects of having Na 2 SO 4 in the initial material) and (2) the production of K 2 SO 4 and NaCl from Na 2 SO 4 and KCl. Section 6 is excerpted from the internet to show some examples of the information available on crystallizers

  12. Applications of thin-film sandwich crystallization platforms

    Energy Technology Data Exchange (ETDEWEB)

    Axford, Danny, E-mail: danny.axford@diamond.ac.uk; Aller, Pierre; Sanchez-Weatherby, Juan; Sandy, James [Diamond Light Source, Harwell Oxford, Didcot OX11 0DE (United Kingdom)

    2016-03-24

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

  13. Liquid Crystal Colloids

    Science.gov (United States)

    Smalyukh, Ivan I.

    2018-03-01

    Colloids are abundant in nature, science, and technology, with examples ranging from milk to quantum dots and the colloidal atom paradigm. Similarly, liquid crystal ordering is important in contexts ranging from biological membranes to laboratory models of cosmic strings and liquid crystal displays in consumer devices. Some of the most exciting recent developments in both of these soft matter fields emerge at their interface, in the fast-growing research arena of liquid crystal colloids. Mesoscale self-assembly in such systems may lead to artificial materials and to structures with emergent physical behavior arising from patterning of molecular order and nano- or microparticles into precisely controlled configurations. Liquid crystal colloids show exceptional promise for new discovery that may impinge on composite material fabrication, low-dimensional topology, photonics, and so on. Starting from physical underpinnings, I review the state of the art in this fast-growing field, with a focus on its scientific and technological potential.

  14. Highly efficient fluorescence sensing with hollow core photonic crystal fibers

    DEFF Research Database (Denmark)

    Smolka, Stephan; Barth, Michael; Benson, Oliver

    2008-01-01

    We investigate hollow core photonic crystal fibers for ultra-sensitive fluorescence detection by selectively infiltrating the central hole with fluorophores. Dye concentrations down to 10(-9) M can be detected using only nanoliter sample volumes.......We investigate hollow core photonic crystal fibers for ultra-sensitive fluorescence detection by selectively infiltrating the central hole with fluorophores. Dye concentrations down to 10(-9) M can be detected using only nanoliter sample volumes....

  15. Single particle measurements of the chemical composition of cirrus ice residue during CRYSTAL-FACE

    Science.gov (United States)

    Cziczo, D. J.; Murphy, D. M.; Hudson, P. K.; Thomson, D. S.

    2004-02-01

    The first real-time, in situ, investigation of the chemical composition of the residue of cirrus ice crystals was performed during July 2002. This study was undertaken on a NASA WB-57F high-altitude research aircraft as part of CRYSTAL-FACE, a field campaign which sought to further our understanding of the relation of clouds, water vapor, and climate by characterizing, among other parameters, anvil cirrus formed about the Florida peninsula. A counter flow virtual impactor (CVI) was used to separate cirrus ice from the unactivated interstitial aerosol particles and evaporate condensed-phase water. Residual material, on a crystal-by-crystal basis, was subsequently analyzed using the NOAA Aeronomy Laboratory's Particle Analysis by Laser Mass Spectrometry (PALMS) instrument. Sampling was performed from 5 to 15 km altitude and from 12° to 28° north latitude within cirrus originating over land and ocean. Chemical composition measurements provided several important results. Sea salt was often incorporated into cirrus, consistent with homogeneous ice formation by aerosol particles from the marine boundary layer. Size measurements showed that large particles preferentially froze over smaller ones. Meteoritic material was found within ice crystals, indicative of a relation between stratospheric aerosol particles and tropospheric clouds. Mineral dust was the dominant residue observed in clouds formed during a dust transport event from the Sahara, consistent with a heterogeneous freezing mechanism. These results show that chemical composition and size are important determinants of which aerosol particles form cirrus ice crystals.

  16. Single Crystal Synthesis and STM Studies of High Temperature Superconductors

    Science.gov (United States)

    Barrientos, Alfonso

    1997-01-01

    This is a final report for the work initiated in September of 1994 under the grant NAG8-1085 - NASA/OMU, on the fabrication of bulk and single crystal synthesis, specific heat measuring and STM studies of high temperature superconductors. Efforts were made to fabricate bulk and single crystals of mercury based superconducting material. A systematic thermal analysis on the precursors for the corresponding oxides and carbonates were carried out to synthesized bulk samples. Bulk material was used as seed in an attempt to grow single crystals by a two-step self flux process. On the other hand bulk samples were characterized by x-ray diffraction, electrical resistivity and magnetic susceptibility, We studied the specific heat behavior in the range from 80 to 300 K. Some preliminary attempts were made to study the atomic morphology of our samples. As part of our efforts we built an ac susceptibility apparatus for measuring the transition temperature of our sintered samples.

  17. Crystallization and demineralization phenomena in washed-rind cheese.

    Science.gov (United States)

    Tansman, Gil F; Kindstedt, Paul S; Hughes, John M

    2017-11-01

    This report documents an observational study of a high-moisture washed-rind cheese. Three batches of cheese were sampled on a weekly basis for 6 wk and again at wk 10. Center, under-rind, rind, and smear samples were tested for pH, moisture, and selected mineral elements. Powder x-ray diffractometry and petrographic microscopy were applied to identify and image the crystal phases. The pH of the rind increased by over 2 pH units by wk 10. The pH of the under-rind increased but remained below the rind pH, whereas the center pH decreased for most of aging and only began to rise after wk 5. Diffractograms of smear material revealed the presence of 4 crystal phases: brushite, calcite, ikaite, and struvite. The phases nucleated in succession over the course of aging, with calcite and ikaite appearing around the same time. A very small amount of brushite appeared sporadically in center and under-rind samples, but otherwise no other crystallization was observed beneath the rind. Micrographs revealed that crystals in the smear grew to over 250 μm in length by wk 10, and at least 2 different crystal phases, probably ikaite and struvite, could be differentiated by their different optical properties. The surface crystallization was accompanied by a mineral diffusion phenomenon that resulted, on average, in a 217, 95.7, and 149% increase in calcium, phosphorus, and magnesium, respectively, in the rind by wk 10. The diffusion phenomenon caused calcium, phosphorus, and magnesium to decrease, on average, by 55.0, 21.5, and 36.3%, respectively, in the center by wk 10. The present study represents the first observation of crystallization and demineralization phenomena in washed-rind cheese. The Authors. Published by the Federation of Animal Science Societies and Elsevier Inc. on behalf of the American Dairy Science Association®. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/3.0/).

  18. Critical points in the Bragg glass phase of a weakly pinned crystal of ...

    Indian Academy of Sciences (India)

    the dynamical annealing of the disordered bundles of vortices injected through the sample edges towards the destined ... weakly pinned crystals of the systems like, 2H-NbSe2 and the cubic (C15) CeRu2. [12]. ... systems. This in turn im- ..... We show in figure 6 an updated version of the vortex phase diagram in the given.

  19. Synthesis of porous CuInS2 crystals using a stirrer

    International Nuclear Information System (INIS)

    Akaki, Yoji; Ohno, Yuki; Momiki, Takanori

    2013-01-01

    Porous CuInS 2 crystals were grown from starting materials CuCl 2 .2H 2 O, InCl 3 .4H 2 O and thiorea with ethylene glycol solution, that were placed into a flask, heated, and refluxed for 1 hour. The diffraction peaks only from CuInS 2 phase appear for all the samples. The morphology of CuInS 2 crystal was porous, and the porous crystals exist in two kinds. One kind was flower-like crystals which complexly lack the flakes, another one was sphere-like crystals existed with a number of the poles. The specific surface area of the samples grown by stirring starting materials with In to Cu ratio of 4.3 for 30 minutes was found approximately to be 55 m 2 /g. (copyright 2013 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  20. Fully automatic characterization and data collection from crystals of biological macromolecules.

    Science.gov (United States)

    Svensson, Olof; Malbet-Monaco, Stéphanie; Popov, Alexander; Nurizzo, Didier; Bowler, Matthew W

    2015-08-01

    Considerable effort is dedicated to evaluating macromolecular crystals at synchrotron sources, even for well established and robust systems. Much of this work is repetitive, and the time spent could be better invested in the interpretation of the results. In order to decrease the need for manual intervention in the most repetitive steps of structural biology projects, initial screening and data collection, a fully automatic system has been developed to mount, locate, centre to the optimal diffraction volume, characterize and, if possible, collect data from multiple cryocooled crystals. Using the capabilities of pixel-array detectors, the system is as fast as a human operator, taking an average of 6 min per sample depending on the sample size and the level of characterization required. Using a fast X-ray-based routine, samples are located and centred systematically at the position of highest diffraction signal and important parameters for sample characterization, such as flux, beam size and crystal volume, are automatically taken into account, ensuring the calculation of optimal data-collection strategies. The system is now in operation at the new ESRF beamline MASSIF-1 and has been used by both industrial and academic users for many different sample types, including crystals of less than 20 µm in the smallest dimension. To date, over 8000 samples have been evaluated on MASSIF-1 without any human intervention.

  1. Studies of the surface structures of molecular crystals and of adsorbed molecular monolayers on the (111) crystal faces of platinum and silver by low-energy electron diffraction

    International Nuclear Information System (INIS)

    Firment, L.E.

    1977-01-01

    The structures of molecular crystal surfaces were investigated for the first time by the use of low-energy electron diffraction (LEED). The experimental results from a variety of molecular crystals were examined and compared as a first step towards understanding the properties of these surfaces on a microscopic level. The method of sample preparation employed, vapor deposition onto metal single-crystal substrates at low temperatures in ultrahigh vacuum, allowed concurrent study of the structures of adsorbed monolayers on metal surfaces and of the growth processes of molecular films on metal substrates. The systems investigated were ice, ammonia, naphthalene, benzene, the n-paraffins (C 3 to C 8 ), cyclohexane, trioxane, acetic acid, propionic acid, methanol, and methylamine adsorbed and condensed on both Pt(111) and Ag(111) surfaces. Electron-beam-induced damage of the molecular surfaces was observed after electron exposures of 10 -4 A sec cm -2 at 20 eV. Aromatic molecular crystal samples were more resistant to damage than samples of saturated molecules. The quality and orientation of the grown molecular crystal films were influenced by substrate preparation and growth conditions. Forty ordered monolayer structures were observed. 110 figures, 22 tables, 162 references

  2. Tunable Crystal-to-Crystal Phase Transition in a Cadmium Halide Chain Polymer

    Directory of Open Access Journals (Sweden)

    Ulli Englert

    2011-07-01

    Full Text Available The chain polymer [{Cd(μ-X2py2}1∞] (X = Cl, Br; py = pyridine undergoes a fully reversible phase transition between a monoclinic low-temperature and an orthorhombic high-temperature phase. The transformation can be directly monitored in single crystals and can be confirmed for the bulk by powder diffraction. The transition temperature can be adjusted by tuning the composition of the mixed-halide phase: Transition temperatures between 175 K up to the decomposition of the material at ca. 350 K are accessible. Elemental analysis, ion chromatography and site occupancy refinements from single-crystal X-ray diffraction agree with respect to the stoichiometric composition of the samples.

  3. Sampling hydrometeors in clouds in-situ - the replicator technique

    Science.gov (United States)

    Wex, Heike; Löffler, Mareike; Griesche, Hannes; Bühl, Johannes; Stratmann, Frank; Schmitt, Carl; Dirksen, Ruud; Reichardt, Jens; Wolf, Veronika; Kuhn, Thomas; Prager, Lutz; Seifert, Patric

    2017-04-01

    For the examination of ice crystals in clouds, concerning their number concentrations, sizes and shapes, often instruments mounted on fast flying aircraft are used. One related disadvantage is possible shattering of the ice crystals on inlets, which has been improved with the introduction of the "Korolev-tip" and by accounting for inter-arrival times (Korolev et al., 2013, 2015), but additionally, the typically fast flying aircraft allow only for a low spatial resolution. Alternative sampling methods have been introduced as e.g., a replicator by Miloshevich & Heymsfield (1997) and an in-situ imager by by Kuhn & Heymsfield (2016). They both sample ice crystals onto an advancing stripe while ascending on a balloon, conserving the ice crystals either in formvar for later off-line analysis under a microscope (Miloshevich & Heymsfield, 1997) or imaging them upon their impaction on silicone oil (Kuhn & Heymsfield, 2016), both yielding vertical profiles for different ice crystal properties. A measurement campaign was performed at the Lindenberg Meteorological Observatory of the German Meteorological Service (DWD) in Germany in October 2016, during which both types of instruments were used during balloon ascents, while ground-based Lidar and cloud-radar measurements were performed simultaneously. The two ice particle sondes were operated by people from the Lulea University of Technology and from TROPOS, where the latter one was made operational only recently. Here, we will show first results of the TROPOS replicator on ice crystals sampled during one ascent, for which the collected ice crystals were analyzed off-line using a microscope. Literature: Korolev, A., E. Emery, and K. Creelman (2013), Modification and tests of particle probe tips to mitigate effects of ice shattering, J. Atmos. Ocean. Tech., 30, 690-708, 2013. Korolev, A., and P. R. Field (2015), Assessment of the performance of the inter-arrival time algorithm to identify ice shattering artifacts in cloud

  4. Fast high-pressure freezing of protein crystals in their mother liquor

    International Nuclear Information System (INIS)

    Burkhardt, Anja; Warmer, Martin; Panneerselvam, Saravanan; Wagner, Armin; Zouni, Athina; Glöckner, Carina; Reimer, Rudolph; Hohenberg, Heinrich; Meents, Alke

    2012-01-01

    Protein crystals were vitrified using high-pressure freezing in their mother liquor at 210 MPa and 77 K without cryoprotectants or oil coating. The method was successfully applied to photosystem II, which is representative of a membrane protein with a large unit cell and weak crystal contacts. High-pressure freezing (HPF) is a method which allows sample vitrification without cryoprotectants. In the present work, protein crystals were cooled to cryogenic temperatures at a pressure of 210 MPa. In contrast to other HPF methods published to date in the field of cryocrystallography, this protocol involves rapid sample cooling using a standard HPF device. The fast cooling rates allow HPF of protein crystals directly in their mother liquor without the need for cryoprotectants or external reagents. HPF was first attempted with hen egg-white lysozyme and cubic insulin crystals, yielding good to excellent diffraction quality. Non-cryoprotected crystals of the membrane protein photosystem II have been successfully cryocooled for the first time. This indicates that the presented HPF method is well suited to the vitrification of challenging systems with large unit cells and weak crystal contacts

  5. Isolation, purification, crystallization and preliminary crystallographic studies of amaryllin, a plant pathogenesis-related protein from Amaryllis belladonna

    International Nuclear Information System (INIS)

    Kumar, Sanjit; Singh, Nagendra; Sinha, Mau; Kaur, Punit; Srinivasan, A.; Sharma, Sujata; Singh, T. P.

    2009-01-01

    A novel 15 kDa antifungal protein amaryllin has been crystallized using 30% PEG 8000 as the precipitating agent. The crystals belong to orthorhombic space group I or I2 1 2 1 2 1 with cell dimensions, a = 48.6, b = 61.9 and c = 79.6–Å. A novel antifungal protein, amaryllin, has been isolated from the underground bulbs of Amaryllis belladonna, purified to homogeneity and crystallized. The protein was extracted using ammonium sulfate fractionation. The purified protein samples indicated a molecular weight of 15 kDa on SDS–PAGE. The protein showed antifungal activity against Aspergillus flavus and Fusarium oxysporum. The N-terminal sequence of the first 15 amino-acid residues was determined using Edman degradation and did not show significant sequence identity to any known protein. The protein was crystallized using the hanging-drop vapour-diffusion method with 30% PEG 8000 as precipitating agent. The crystals diffracted to 2.7 Å resolution and belonged to the orthorhombic space group I222 or I2 1 2 1 2 1 , with unit-cell parameters a = 48.6, b = 61.9, c = 79.6 Å. The complete sequence and structure determination of amaryllin are in progress

  6. Scintillation and optical properties of Ce{sup 3+}-doped CaGdAl{sub 3}O{sub 7} single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Mori, Masaki, E-mail: masaki.mori.mz4@ms.naist.jp [Graduate School of Materials Science, Nara Institute of Science and Technology (NAIST), 8916-5 Takayama-cho, Ikoma-shi, Nara 630-0192 (Japan); Nakauchi, Daisuke; Okada, Go [Graduate School of Materials Science, Nara Institute of Science and Technology (NAIST), 8916-5 Takayama-cho, Ikoma-shi, Nara 630-0192 (Japan); Fujimoto, Yutaka [Department of Applied Chemistry, Graduate School of Engineering, Tohoku University, 6-6-07 Aoba, Aramaki, Aoba-ku, Sendai, 980-8579 (Japan); Kawaguchi, Noriaki [Graduate School of Materials Science, Nara Institute of Science and Technology (NAIST), 8916-5 Takayama-cho, Ikoma-shi, Nara 630-0192 (Japan); Koshimizu, Masanori [Department of Applied Chemistry, Graduate School of Engineering, Tohoku University, 6-6-07 Aoba, Aramaki, Aoba-ku, Sendai, 980-8579 (Japan); Yanagida, Takayuki [Graduate School of Materials Science, Nara Institute of Science and Technology (NAIST), 8916-5 Takayama-cho, Ikoma-shi, Nara 630-0192 (Japan)

    2017-06-15

    The single crystals of 0, 0.6, 1, 1.6 and 2 mol% Ce doped CaGdAl{sub 3}O{sub 7} (Ce:CGAM) were grown by the Floating Zone method, and investigated on photoluminescence (PL) and scintillation properties. In the PL spectra, a broad emission appeared over 380–500 nm under 280 and 360 nm excitations with the quantum yield of 33.8–38.8%. Under a vacuum ultraviolet excitation (90 nm) using a synchrotron source, non-doped CGAM single crystal showed broad emissions over 250–650 nm. The PL decay time profiles followed a monotonic exponential decay with a decay time constant of around 33 ns. The scintillation spectra were similar to those of PL. All of the samples exhibited a clear photoabsorption peak and Compton edge in the pulse height spectra measured under {sup 137}Cs γ-ray irradiation, and the absolute scintillation light yield (LY) was highest for the 2% Ce-doped sample with the value of 3300±300 ph/MeV. The scintillation decay profiles were approximated by a third order exponential decay function, and the extracted decay time of Ce{sup 3+} emission component was around 36–44 ns. Among all the samples, 2%Ce:CGAM single crystal sample showed the best afterglow level as a scintillator under X-ray irradiation. - Highlights: •Ce{sup 3+}-doped CaGdAl{sub 3}O{sub 7} single crystals were synthesized by the FZ method. •Optical and scintillation properties of Ce{sup 3+}-doped CaGdAl{sub 3}O{sub 7} were investigated. •Photoabsorption peak in a pulse height spectrum was clearly observed under γ-rays.

  7. Crystal ball single event display

    International Nuclear Information System (INIS)

    Grosnick, D.; Gibson, A.; Allgower, C.; Alyea, J.; Argonne National Lab., IL

    1997-01-01

    The Single Event Display (SED) is a routine that is designed to provide information graphically about a triggered event within the Crystal Ball. The SED is written entirely in FORTRAN and uses the CERN-based HICZ graphing package. The primary display shows the amount of energy deposited in each of the NaI crystals on a Mercator-like projection of the crystals. Ten different shades and colors correspond to varying amounts of energy deposited within a crystal. Information about energy clusters is displayed on the crystal map by outlining in red the thirteen (or twelve) crystals contained within a cluster and assigning each cluster a number. Additional information about energy clusters is provided in a series of boxes containing useful data about the energy distribution among the crystals within the cluster. Other information shown on the event display include the event trigger type and data about π o 's and η's formed from pairs of clusters as found by the analyzer. A description of the major features is given, along with some information on how to install the SED into the analyzer

  8. Radiation induced color in topaz crystals

    International Nuclear Information System (INIS)

    Castagnet, A.C.; Rocca, H.C.C.; Rostilato, M.E.C.M.

    1989-08-01

    The presence of defects and impurities in the crystal lattice alters the eletric field distribution within the crystal, allowing the electrons to occupy energy levels in the forbbiden band. Ionizing radiation supply the required energy to permit the electrons originaly bound to lattice atoms, to occupy effectively those intermediate levels, forming color centers. Dependig upon the nature and energy of the radiation, it is possible to produce defects in regions of the crystal, generating color centers. Based on these premises, a technique to induce color in originally colorless topaz, by using the IEA-R1 nuclear reactor, was developed at Engineering and Industrial Application Department (TE). Samples were irradiated inside iron capsules coated with cadmium foils. The iron, and principaly the cadmium, absorb the thermal neutrons that could activate crystal impurities generating long-lived radioisotopes. The epithermal neutrons that overpass the iron and cadmium barriers interact with the crystal atoms, causing lattice defects which give rise to color center, by subsequent ionization processes. The procedure used at TE induces permanent blue color, in natural colorless topaz. (author) [pt

  9. Inorganic elements in sugar samples

    International Nuclear Information System (INIS)

    Salles, Paulo M.B. de; Campos, Tarcisio P.R. de

    2013-01-01

    Sugar is considered a safe food ingredient; however, it can be contaminated by organic elements since its planting until its production process. Thus, this study aims at checking the presence of inorganic elements in samples of crystal, refined and brown sugar available for consumption in Brazil. The applied technique was neutron activation analysis, the k 0 method, using the TRIGA MARK - IPR-R1 reactor located at CDTN/CNEN, in Belo Horizonte. It was identified the presence of elements such as, Au, Br, Co, Cr, Hf, K, Na, Sb, Sc and Zn in the samples of crystal/refined sugar and the presence of As, Au, Br, Ca, Co, Cr, Cs, Fe, Hf, K, Na, Sb, Sc, Sm, Sr, Th and Zn in the brown sugar samples. The applied technique was appropriate to this study because it was not necessary to put the samples in solution, essential condition in order to apply other techniques, avoiding contaminations and sample losses, besides allowing a multi elementary detection in different sugar samples. (author)

  10. Inorganic elements in sugar samples

    Energy Technology Data Exchange (ETDEWEB)

    Salles, Paulo M.B. de; Campos, Tarcisio P.R. de, E-mail: pauladesalles@yahoo.com.br, E-mail: tprcampos@pq.cnpq.br [Universidade Federal de Minas Gerais (DEN/UFMG), Belo Horizonte, MG (Brazil). Departamento de Engenharia Nuclear; Menezes, Maria Angela de B.C., E-mail: menezes@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2013-07-01

    Sugar is considered a safe food ingredient; however, it can be contaminated by organic elements since its planting until its production process. Thus, this study aims at checking the presence of inorganic elements in samples of crystal, refined and brown sugar available for consumption in Brazil. The applied technique was neutron activation analysis, the k{sub 0} method, using the TRIGA MARK - IPR-R1 reactor located at CDTN/CNEN, in Belo Horizonte. It was identified the presence of elements such as, Au, Br, Co, Cr, Hf, K, Na, Sb, Sc and Zn in the samples of crystal/refined sugar and the presence of As, Au, Br, Ca, Co, Cr, Cs, Fe, Hf, K, Na, Sb, Sc, Sm, Sr, Th and Zn in the brown sugar samples. The applied technique was appropriate to this study because it was not necessary to put the samples in solution, essential condition in order to apply other techniques, avoiding contaminations and sample losses, besides allowing a multi elementary detection in different sugar samples. (author)

  11. Temperature-mediated polymorphism in molecular crystals: The impact on crystal packing and charge transport

    KAUST Repository

    Stevens, Loah A.; Goetz, Katelyn P.; Fonari, Alexandr; Shu, Ying; Williamson, Rachel M.; Bredas, Jean-Luc; Coropceanu, Veaceslav P.; Jurchescu, Oana D.; Collis, Gavin E.

    2015-01-01

    We report a novel synthesis to ultra high purity 7,14-bis((trimethylsilyl)ethynyl)dibenzo[b,def]-chrysene (TMS-DBC) and the use of this material in the growth of single crystals by solution and vapor deposition techniques. We observe that the substrate temperature has a dramatic impact on the crystal growth, producing two distinct polymorphs of TMS-DBC; low temperature (LT) fine red needles and high temperature (HT) large yellow platelets. Single crystal X-ray crystallography confirms packing structures where the LT crystals form a 1D slipped-stack structure, while the HT crystals adopt a 2D brickwork motif. These polymorphs also represent a rare example where both are extremely stable and do not interconvert to the other crystal structure upon solvent or thermal annealing. Single crystal organic field-effect transistors of the LT and HT crystals show that the HT 2D brickwork motif produces hole mobilities as high as 2.1 cm2 V-1 s-1, while the mobility of the 1D structure is significantly lower, at 0.028 cm2 V-1 s-1. Electronic-structure calculations indicate that the superior charge transport in the brickwork polymorph in comparison to the slipped-stack polymorph is due to the presence of an increased dimensionality of the charge migration pathways.

  12. Temperature-mediated polymorphism in molecular crystals: The impact on crystal packing and charge transport

    KAUST Repository

    Stevens, Loah A.

    2015-01-13

    We report a novel synthesis to ultra high purity 7,14-bis((trimethylsilyl)ethynyl)dibenzo[b,def]-chrysene (TMS-DBC) and the use of this material in the growth of single crystals by solution and vapor deposition techniques. We observe that the substrate temperature has a dramatic impact on the crystal growth, producing two distinct polymorphs of TMS-DBC; low temperature (LT) fine red needles and high temperature (HT) large yellow platelets. Single crystal X-ray crystallography confirms packing structures where the LT crystals form a 1D slipped-stack structure, while the HT crystals adopt a 2D brickwork motif. These polymorphs also represent a rare example where both are extremely stable and do not interconvert to the other crystal structure upon solvent or thermal annealing. Single crystal organic field-effect transistors of the LT and HT crystals show that the HT 2D brickwork motif produces hole mobilities as high as 2.1 cm2 V-1 s-1, while the mobility of the 1D structure is significantly lower, at 0.028 cm2 V-1 s-1. Electronic-structure calculations indicate that the superior charge transport in the brickwork polymorph in comparison to the slipped-stack polymorph is due to the presence of an increased dimensionality of the charge migration pathways.

  13. Control of liquid crystal molecular orientation using ultrasound vibration

    Energy Technology Data Exchange (ETDEWEB)

    Taniguchi, Satoki [Faculty of Life and Medical Sciences, Doshisha University, 1-3 Tataramiyakodani, Kyotanabe, Kyoto 610-0321 (Japan); Wave Electronics Research Center, Doshisha University, 1-3 Tataramiyakodani, Kyotanabe, Kyoto 610-0321 (Japan); Koyama, Daisuke; Matsukawa, Mami [Wave Electronics Research Center, Doshisha University, 1-3 Tataramiyakodani, Kyotanabe, Kyoto 610-0321 (Japan); Faculty of Science and Engineering, Doshisha University, 1-3 Tataramiyakodani, Kyotanabe, Kyoto 610-0321 (Japan); Shimizu, Yuki; Emoto, Akira [Faculty of Science and Engineering, Doshisha University, 1-3 Tataramiyakodani, Kyotanabe, Kyoto 610-0321 (Japan); Nakamura, Kentaro [Precision and Intelligence Laboratory, Tokyo Institute of Technology, 4259-R2-26, Nagatsuta-cho, Midori-ku, Yokohama 226-8503 (Japan)

    2016-03-07

    We propose a technique to control the orientation of nematic liquid crystals using ultrasound and investigate the optical characteristics of the oriented samples. An ultrasonic liquid crystal cell with a thickness of 5–25 μm and two ultrasonic lead zirconate titanate transducers was fabricated. By exciting the ultrasonic transducers, the flexural vibration modes were generated on the cell. An acoustic radiation force to the liquid crystal layer was generated, changing the molecular orientation and thus the light transmission. By modulating the ultrasonic driving frequency and voltage, the spatial distribution of the molecular orientation of the liquid crystals could be controlled. The distribution of the transmitted light intensity depends on the thickness of the liquid crystal layer because the acoustic field in the liquid crystal layer is changed by the orientational film.

  14. An affine microsphere approach to modeling strain-induced crystallization in rubbery polymers

    Science.gov (United States)

    Nateghi, A.; Dal, H.; Keip, M.-A.; Miehe, C.

    2018-01-01

    Upon stretching a natural rubber sample, polymer chains orient themselves in the direction of the applied load and form crystalline regions. When the sample is retracted, the original amorphous state of the network is restored. Due to crystallization, properties of rubber change considerably. The reinforcing effect of the crystallites stiffens the rubber and increases the crack growth resistance. It is of great importance to understand the mechanism leading to strain-induced crystallization. However, limited theoretical work has been done on the investigation of the associated kinetics. A key characteristic observed in the stress-strain diagram of crystallizing rubber is the hysteresis, which is entirely attributed to strain-induced crystallization. In this work, we propose a micromechanically motivated material model for strain-induced crystallization in rubbers. Our point of departure is constructing a micromechanical model for a single crystallizing polymer chain. Subsequently, a thermodynamically consistent evolution law describing the kinetics of crystallization on the chain level is proposed. This chain model is then incorporated into the affine microsphere model. Finally, the model is numerically implemented and its performance is compared to experimental data.

  15. Calcium oxalate crystals: an integral component of the Sclerotinia sclerotiorum/Brassica carinata pathosystem.

    Directory of Open Access Journals (Sweden)

    Margaret B Uloth

    Full Text Available Oxalic acid is an important virulence factor for disease caused by the fungal necrotrophic pathogen Sclerotinia sclerotiorum, yet calcium oxalate (CaOx crystals have not been widely reported. B. carinata stems were infected with S. sclerotiorum and observed using light microscopy. Six hours post inoculation (hpi, CaOx crystals were evident on 46% of stem sections and by 72 hpi on 100%, demonstrating that the secretion of oxalic acid by S. sclerotiorum commences before hyphal penetration. This is the first time CaOx crystals have been reported on B. carinata infected with S. sclerotiorum. The shape of crystals varied as infection progressed. Long tetragonal rods were dominant 12 hpi (68% of crystal-containing samples, but by 72 hpi, 50% of stems displayed bipyramidal crystals, and only 23% had long rods. Scanning electron microscopy from 24 hpi revealed CaOx crystals in all samples, ranging from tiny irregular crystals (< 0.5 μm to large (up to 40 μm highly organized arrangements. Crystal morphology encompassed various forms, including tetragonal prisms, oval plates, crystal sand, and druses. Large conglomerates of CaOx crystals were observed in the hyphal mass 72 hpi and these are proposed as a strategy of the fungus to hold and detoxify Ca2+ions. The range of crystal morphologies suggests that S. sclerotiorum growth and infection controls the form taken by CaOx crystals.

  16. Co-doped sodium chloride crystals exposed to different irradiation temperature

    Energy Technology Data Exchange (ETDEWEB)

    Ortiz-Morales, A. [Unidad Profesional Interdisciplinaria de Ingenieria y Tecnologias Avanzadas, IPN, Av. Instituto Politecnico Nacional 2580, Col. La Laguna Ticoman, 07340 Mexico D.F., Mexico and Unidad de Irradiacion y Segurid (Mexico); Cruz-Zaragoza, E.; Furetta, C. [Unidad de Irradiacion y Seguridad Radiologica, Instituto de Ciencias Nucleares, Universidad Nacional Autonoma de Mexico, A.P. 70-543, 04510 Mexico D.F (Mexico); Kitis, G. [Nuclear Physics Laboratory, Aristotle University of Thessaloniki, Thessaloniki 54124 (Greece); Flores J, C.; Hernandez A, J.; Murrieta S, H. [Instituto de Fisica, Universidad Nacional Autonoma de Mexico, AP. 20-364, 01000 Mexico D.F (Mexico)

    2013-07-03

    Monocrystals of NaCl:XCl{sub 2}:MnCl{sub 2}(X = Ca,Cd) at four different concentrations have been analyzed. The crystals were exposed to different irradiation temperature, such as at room temperature (RT), solid water (SW), dry ice (DI) and liquid nitrogen (LN). The samples were irradiated with photon from {sup 60}Co irradiators. The co-doped sodium chloride crystals show a complex structure of glow curves that can be related to different distribution of traps. The linearity response was analyzed with the F(D) index. The F(D) value was less than unity indicating a sub-linear response was obtained from the TL response on the function of the dose. The glow curves were deconvoluted by using the CGCD program based on the first, second and general order kinetics.

  17. The Kinetics of Crystallization of Colloids and Proteins: A Light Scattering Study

    Science.gov (United States)

    McClymer, Jim

    2002-01-01

    Hard-sphere colloidal systems serve as model systems for aggregation, nucleation, crystallization and gelation as well as interesting systems in their own right.There is strong current interest in using colloidal systems to form photonic crystals. A major scientific thrust of NASA's microgravity research is the crystallization of proteins for structural determination. The crystallization of proteins is a complicated process that requires a great deal of trial and error experimentation. In spite of a great deal of work, "better" protein crystals cannot always be grown in microgravity and conditions for crystallization are not well understood. Crystallization of colloidal systems interacting as hard spheres and with an attractive potential induced by entropic forces have been studied in a series of static light scattering experiments. Additionally, aggregation of a protein as a function of pH has been studied using dynamic light scattering. For our experiments we used PMMA (polymethylacrylate) spherical particles interacting as hard spheres, with no attractive potential. These particles have a radius of 304 nanometers, a density of 1.22 gm/ml and an index of refraction of 1.52. A PMMA colloidal sample at a volume fraction of approximately 54% was index matched in a solution of cycloheptyl bromide (CHB) and cis-decalin. The sample is in a glass cylindrical vial that is placed in an ALV static and dynamic light scattering goniometer system. The vial is immersed in a toluene bath for index matching to minimize flair. Vigorous shaking melts any colloidal crystals initially present. The sample is illuminated with diverging laser light (632.8 nanometers) from a 4x microscope objective placed so that the beam is approximately 1 cm in diameter at the sample location. The sample is rotated about its long axis at approximately 3.5 revolutions per minute (highest speed) as the colloidal crystal system is non-ergodic. The scattered light is detected at various angles using the

  18. Electrically Anisotropic Layered Perovskite Single Crystal

    KAUST Repository

    Li, Ting-You

    2016-04-01

    Organic-inorganic hybrid perovskites (OIHPs), which are promising materials for electronic and optoelectronic applications (1-10), have made into layered organic-inorganic hybrid perovskites (LOIHPs). These LOIHPs have been applied to thin-film transistors, solar cells and tunable wavelength phosphors (11-18). It is known that devices fabricated with single crystal exhibit the superior performance, which makes the growth of large-sized single crystals critical for future device applications (19-23). However, the difficulty in growing large-sized LOIHPs single crystal with superior electrical properties limits their practical applications. Here, we report a method to grow the centimeter-scaled LOIHP single crystal of [(HOC2H4NH3)2PbI4], demonstrating the potentials in mass production. After that, we reveal anisotropic electrical and optoelectronic properties which proved the carrier propagating along inorganic framework. The carrier mobility of in-inorganic-plane (in-plane) devices shows the average value of 45 cm2 V–1 s–1 which is about 100 times greater than the record of LOIHP devices (15), showing the importance of single crystal in device application. Moreover, the LOIHP single crystals show its ultra-short carrier lifetime of 42.7 ps and photoluminescence quantum efficiency (PLQE) of 25.4 %. We expect this report to be a start of LOIHPs for advanced applications in which the anisotropic properties are needed (24-25), and meets the demand of high-speed applications and fast-response applications.

  19. The effect of UV exposure and heat treatment on crystallization behavior of photosensitive glasses

    Science.gov (United States)

    Kıbrıslı, Orhan; Ersundu, Ali Erçin

    2018-05-01

    In this study, photosensitive glasses in the Na2O-ZnO-Al2O3-SiO2 system with photosensitizing agents (cerium, silver, tin, antimony) and halogenides (NaF and KBr) were synthesized through a conventional melt-quenching technique. The crystallization mechanism was investigated for solely heat-treated and UV-exposed + heat-treated samples using differential thermal analysis (DTA), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS) and scanning electron microscopy (SEM) techniques to understand the effect of UV exposure on crystallization behavior of photosensitive glasses. Accordingly, non-isothermal DTA measurements were performed at different heating rates to determine crystallization peak, T p, and onset, T c, temperatures. For solely heat-treated samples, the kinetic parameters such as the Avrami constant, n, and morphology index, m, were calculated as 1 from the Ozawa method indicating surface crystallization and the value of crystallization activation energy was calculated as 944 kJ/mol using modified Kissinger method. On the contrary, bulk crystallization was found to be predominant for UV exposed + heat-treated samples revealing that UV exposure is the primary cause of bulk crystallization in photosensitive glasses.

  20. Surface crystallization and magnetic properties of amorphous Fe80B20 alloy

    International Nuclear Information System (INIS)

    Vavassori, P.; Ronconi, F.; Puppin, E.

    1997-01-01

    We have studied the effects of surface crystallization on the magnetic properties of Fe 80 B 20 amorphous alloys. The surface magnetic properties have been studied with magneto-optic Kerr measurements, while those of bulk with a vibrating sample magnetometer. This study reveals that surface crystallization is similar to the bulk process but occurs at a lower temperature. At variance with previous results on other iron-based amorphous alloys the surface crystalline layer does not induce bulk magnetic hardening. Furthermore, both the remanence to saturation ratio and the bulk magnetic anisotropy do not show appreciable variations after the formation of the surface crystalline layer. The Curie temperature of the surface layer is lower with respect to the bulk of the sample. These effects can be explained by a lower boron concentration in the surface region of the as-cast amorphous alloy. Measurements of the chemical composition confirm a reduction of boron concentration in the surface region. copyright 1997 American Institute of Physics

  1. Crystallization process and magnetic properties of amorphous iron oxide nanoparticles

    International Nuclear Information System (INIS)

    Phu, N D; Luong, N H; Chau, N; Hai, N H; Ngo, D T; Hoang, L H

    2011-01-01

    This paper studied the crystallization process, phase transition and magnetic properties of amorphous iron oxide nanoparticles prepared by the microwave heating technique. Thermal analysis and magnetodynamics studies revealed many interesting aspects of the amorphous iron oxide nanoparticles. The as-prepared sample was amorphous. Crystallization of the maghemite γ-Fe 2 O 3 (with an activation energy of 0.71 eV) and the hematite α-Fe 2 O 3 (with an activation energy of 0.97 eV) phase occurred at around 300 deg. C and 350 deg. C, respectively. A transition from the maghemite to the hematite occurred at 500 deg. C with an activation energy of 1.32 eV. A study of the temperature dependence of magnetization supported the crystallization and the phase transformation. Raman shift at 660 cm -1 and absorption band in the infrared spectra at 690 cm -1 showed the presence of disorder in the hematite phase on the nanoscale which is supposed to be the origin of the ferromagnetic behaviour of that antiferromagnetic phase.

  2. Role of crystal orientation on chemical mechanical polishing of single crystal copper

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Aibin, E-mail: abzhu@mail.xjtu.edu.cn; He, Dayong; Luo, Wencheng; Liu, Yangyang

    2016-11-15

    Highlights: • The role of crystal orientation in cooper CMP by quasi-continuum was studied. • The atom displacement diagrams were obtained and analyzed. • The stress distribution diagrams and load-displacement curves were analyzed. • This research is helpful to revealing the material removal mechanism of CMP. - Abstract: The material removal mechanism of single crystal copper in chemical mechanical polishing (CMP) has not been intensively investigated. And the role of crystal orientation in CMP of single crystal cooper is not quite clear yet. Quasi-continuum method was adopted in this paper to simulate the process of nano-particles grinding on single crystal copper in CMP process. Three different crystal orientations, i.e. x[100]y[001], x[001]y[110] and x[–211]y[111], were chosen for analysis. The atom displacement diagrams, stress distribution diagrams and load-displacement curves were obtained. After analyzing the deformation mechanism, residual stress of the work piece material and cutting force, results showed that, the crystal orientation of work piece has great influence on the deformation characteristics and surface quality of work piece during polishing. In the A(001)[100] orientation, the residual stress distribution after polishing is deeper, and the stress is larger than that in the B(110)[001] and C(111)[–211] orientations. And the average tangential cutting force in the A(001)[100] orientation is much larger than those in the other two crystal orientation. This research is helpful to revealing the material removal mechanism of CMP process.

  3. Channeling implantation of high energy carbon ions in a diamond crystal: Determination of the induced crystal amorphization

    Science.gov (United States)

    Erich, M.; Kokkoris, M.; Fazinić, S.; Petrović, S.

    2018-02-01

    This work reports on the induced diamond crystal amorphization by 4 MeV carbon ions implanted in the 〈1 0 0〉 oriented crystal and its determination by application of RBS/C and EBS/C techniques. The spectra from the implanted samples were recorded for 1.2, 1.5, 1.75 and 1.9 MeV protons. For the two latter ones the strong resonance of the nuclear elastic scattering 12C(p,p0)12C at 1.737 MeV was explored. The backscattering channeling spectra were successfully fitted and the ion beam induced crystal amorphization depth profile was determined using a phenomenological approach, which is based on the properly defined Gompertz type dechanneling functions for protons in the 〈1 0 0〉 diamond crystal channels and the introduction of the concept of ion beam amorphization, which is implemented through our newly developed computer code CSIM.

  4. Non-Linear Optical Studies On Sol-Gel Derived Lead Chloride Crystals Using Z-Scan Technique

    OpenAIRE

    Rejeena, I; Lillibai, B; Toms, Roseleena; Nampoori, VP N; Radhakrishnan, P

    2014-01-01

    In this paper we report the preparation, optical characterization and non linear optical behavior of pure lead chloride crystals. Lead chloride samples subjected to UV and IR irradiation and electric and magnetic fields have also been investigated Optical nonlinearity in these lead chloride samples were determined using single beam and high sensitive Z-scan technique. Non linear optical studies of these materials in single distilled water show reverse saturable absorption which makes th...

  5. 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

  6. Solubility and crystallization of piroxicam from different solvents in evaporative and cooling crystallizations

    DEFF Research Database (Denmark)

    Qu, Haiyan; Ostergaard, Iben

    2018-01-01

    polarities; It has been found that the solubility of piroxicam in the solvents is in the following order: chloroform > dichloromethane > acetone > ethyl acetate > acetonitrile > acetic acid > methanol > hexane. Crystallization of piroxicam from different solvents has been performed with evaporative.......Results obtained in the present work showed the stochastic nature of nucleation of different polymorphs as well as the complexity of the crystallization of a polymorphic system....

  7. Origin of colossal dielectric permittivity of rutile Ti₀.₉In₀.₀₅Nb₀.₀₅O₂: single crystal and polycrystalline.

    Science.gov (United States)

    Song, Yongli; Wang, Xianjie; Sui, Yu; Liu, Ziyi; Zhang, Yu; Zhan, Hongsheng; Song, Bingqian; Liu, Zhiguo; Lv, Zhe; Tao, Lei; Tang, Jinke

    2016-02-12

    In this paper, we investigated the dielectric properties of (In + Nb) co-doped rutile TiO2 single crystal and polycrystalline ceramics. Both of them showed colossal, up to 10(4), dielectric permittivity at room temperature. The single crystal sample showed one dielectric relaxation process with a large dielectric loss. The voltage-dependence of dielectric permittivity and the impedance spectrum suggest that the high dielectric permittivity of single crystal originated from the surface barrier layer capacitor (SBLC). The impedance spectroscopy at different temperature confirmed that the (In + Nb) co-doped rutile TiO2 polycrystalline ceramic had semiconductor grains and insulating grain boundaries, and that the activation energies were calculated to be 0.052 eV and 0.35 eV for grain and grain boundary, respectively. The dielectric behavior and impedance spectrum of the polycrystalline ceramic sample indicated that the internal barrier layer capacitor (IBLC) mode made a major contribution to the high ceramic dielectric permittivity, instead of the electron-pinned defect-dipoles.

  8. Structure of initial crystals formed during human amelogenesis

    Science.gov (United States)

    Cuisinier, F. J. G.; Voegel, J. C.; Yacaman, J.; Frank, R. M.

    1992-02-01

    X-ray diffraction analysis revealed only the existence of carbonated hydroxyapatite (c.HA) during amelogenesis, whereas conventional transmission electron microscopy investigations showed that developing enamel crystals have a ribbon-like habit. The described compositional changes could be an indication for the presence of minerals different from c.HA. However, the absence of identification of such a mineral shows the need of studies by high resolution electron microscopy (HREM) of initial formed human enamel crystals. We demonstrate the existence of two crystal families involved in the early stages of biomineralization: (a) nanometer-size particles which appeared as a precursor phase; (b) ribbon-like crystals, with a structure closely related to c.HA, which by a progressive thickening process tend to attain the mature enamel crystal habit.

  9. Single-crystal films of a combination of materials (co-crystal) involving DAST and IR-125 for electro-optic applications

    Science.gov (United States)

    Narayanan, A.; Titus, J.; Rajagopalan, H.; Vippa, P.; Thakur, M.

    2006-03-01

    Single-crystal film of DAST (4'-dimethylamino-N-methyl-4-stilbazolium tosylate) has been shown [1] to have exceptionally large electro-optic coefficients (r11 ˜ 770 pm/V at 633 nm). In this report, single crystal film of a combination of materials (co-crystal) involving DAST and a dye molecule IR-125 will be discussed. Modified shear method was used to prepare the co-crystal films. The film has been characterized using polarized optical microscopy, optical absorption spectroscopy and x-ray diffraction. The optical absorption spectrum has two major bands: one at about 350--600 nm corresponding to DAST and the other at about 600-900 nm corresponding to IR-125. The x-ray diffraction results show peaks involving the presence of DAST and IR-125 within the co-crystal film. Since the co-crystal has strong absorption at longer wavelengths it is expected to show higher electro-optic coefficients at longer wavelengths. Preliminary measurements at 1.55 μm indicate a high electro-optic coefficient of the co-crystal film. [1] Swamy, Kutty, Titus, Khatavkar, Thakur, Appl. Phys. Lett. 2004, 85, 4025; Kutty, Thakur, Appl. Phys. Lett. 2005, 87, 191111.

  10. Crystal orientation mapping applied to the Y-TZP/WC composite

    CERN Document Server

    Faryna, M; Sztwiertnia, K

    2002-01-01

    Crystal orientation measurements made by electron backscattered diffraction (EBSD) in the scanning electron microscope (SEM) and microscopic observations provided the basis for a quantitative investigation of microstructure in an yttria stabilized, tetragonal zirconia-based (Y-TZP) composite. Automatic crystal orientation mapping (ACOM) in a SEM can be preferable to transmission electron microscopy (TEM) for microstructural characterization, since no sample thinning is required, extensive crystal data is already available, and the analysis area is greatly increased. A composite with a 20 vol.% tungsten carbide (WC) content was chosen since it revealed crystal relationships between the matrix and carbide phase already established by TEM analysis. However, this composite was difficult to investigate in the EBSD/ SEM since it is non-conductive, the Y-TZP grain size is of the order of the system resolution, and the sample surface, though carefully prepared, reveals a distinctive microtopography. In this paper, so...

  11. Gentle, fast and effective crystal soaking by acoustic dispensing.

    Science.gov (United States)

    Collins, Patrick M; Ng, Jia Tsing; Talon, Romain; Nekrosiute, Karolina; Krojer, Tobias; Douangamath, Alice; Brandao-Neto, Jose; Wright, Nathan; Pearce, Nicholas M; von Delft, Frank

    2017-03-01

    The steady expansion in the capacity of modern beamlines for high-throughput data collection, enabled by increasing X-ray brightness, capacity of robotics and detector speeds, has pushed the bottleneck upstream towards sample preparation. Even in ligand-binding studies using crystal soaking, the experiment best able to exploit beamline capacity, a primary limitation is the need for gentle and nontrivial soaking regimens such as stepwise concentration increases, even for robust and well characterized crystals. Here, the use of acoustic droplet ejection for the soaking of protein crystals with small molecules is described, and it is shown that it is both gentle on crystals and allows very high throughput, with 1000 unique soaks easily performed in under 10 min. In addition to having very low compound consumption (tens of nanolitres per sample), the positional precision of acoustic droplet ejection enables the targeted placement of the compound/solvent away from crystals and towards drop edges, allowing gradual diffusion of solvent across the drop. This ensures both an improvement in the reproducibility of X-ray diffraction and increased solvent tolerance of the crystals, thus enabling higher effective compound-soaking concentrations. The technique is detailed here with examples from the protein target JMJD2D, a histone lysine demethylase with roles in cancer and the focus of active structure-based drug-design efforts.

  12. Properties of laser-crystallized polycrystalline SiGe thin films

    Energy Technology Data Exchange (ETDEWEB)

    Weizman, Moshe

    2008-06-06

    In this thesis, structural, electrical, and optical properties of laser-crystallized polycrystalline Si{sub 1-x}Ge{sub x} thin films with 0crystallization of amorphous Si{sub 1-x}Ge{sub x} thin films with 0.3samples that are exposed to a single laser pulse exhibit a ripple structure that evolves into a hillock structure when the samples are irradiated with additional laser pulses. - It is maintained that the main mechanism behind the structure formation is an instability of the propagating solid-liquid interface during solidification. - The study of defects with electron spin resonance showed that laser-crystallized poly-Si{sub 1-x}Ge{sub x} thin films with 0crystallization method and Ge content. The defect density for solid-phase crystallized SiGe films was lower and amounted to N{sub s}=7 x 10{sup 17} cm{sup -3}. - Germanium-rich laser-crystallized poly-SiGe thin films exhibited mostly a broad atypical electric dipole spin resonance (EDSR) signal that was accompanied by a nearly temperature-independent electrical conductivity in the range 20-100 K. - Most likely, the origin of the grain boundary conductance is due to dangling-bond defects and not impurities. Metallic-like conductance occurs when the dangling-bond defect density is above a critical value of about N{sub C} {approx} 10{sup 18} cm{sup -3}. - Laser crystallized poly-Si{sub 1-x}Ge{sub x} thin films with x{>=}0.5 exhibit optical absorption behavior that is characteristic for disordered SiGe, implying that the absorption occurs primarily at the grain boundaries. A sub-band-gap absorption peak was found for

  13. Effect of sintering on crystallization and structural properties of soda lime silica glass

    Directory of Open Access Journals (Sweden)

    Zaid Mohd Hafiz Mohd

    2017-01-01

    Full Text Available The effect of sintering temperatures on crystallization and structural of the soda lime silica (SLS glass was reported. Elemental weight composition of the SLS glass powder was identified through Energy dispersive X-ray fluorescence (EDXRF analysis while the thermal behavior of the glass was determined using Differential thermal analysis (DTA technique. Archimedes’ method and direct geometric measurement were respectively used to determine bulk density and linear shrinkage of the glass samples. Crystallisation behavior of the samples was investigated by X-ray diffraction (XRD analysis and chemical bonds present in the samples were measured using Fourier Transform Infrared (FTIR spectroscopy. Results showed an increase in the density and linear shrinkage of the samples as a function of the sintering temperature. The XRD analysis revealed the formation of α-quartz (SiO2 and a minor amount of devitrite phases in the samples and these were further verified through the detection of chemical bonds by FTIR after sintering at 800ºC. The properties of the glass-ceramics can be explained on the basis of crystal chemistry which indicated that the alkali ions formed as carriers in the random network structure and can be recommended for the manufacture of glass fiber or toughened glass-ceramic insulators.

  14. Lower-temperature crystallization of CoFeB in MgO magnetic tunnel junctions by using Ti capping layer

    International Nuclear Information System (INIS)

    Ibusuki, Takahiro; Miyajima, Toyoo; Umehara, Shinjiro; Eguchi, Shin; Sato, Masashige

    2009-01-01

    Effects of capping materials on magnetoresistance (MR) properties of MgO magnetic tunnel junctions (MTJs) with a CoFeB free layer were investigated. MR ratios of samples with various capping materials showed a difference in annealing temperature dependence. MTJ with a Ti capping layer annealed at 270 deg. C showed a MR ratio 1.4 times greater than that with a conventional Ta or Ru capping layer. Secondary ion mass spectroscopy and high-resolution transmission electron microscopy images revealed that crystallization of CoFeB was remarkably affected by adjacent materials and the Ti capping layer adjoining CoFeB acted as a boron-absorption layer. These results suggest that the crystallization process can be controlled by choosing proper capping materials. Ti is one of the effective materials that accelerate the crystallization of CoFeB layers at lower annealing temperature

  15. Effect of process parameters on crystal size and morphology of lactose in ultrasound-assisted crystallization

    Energy Technology Data Exchange (ETDEWEB)

    Patel, S.R.; Murthy, Z.V.P. [Chemical Engineering Department, S.V. National Institute of Technology, Surat - 395 007, Gujarat (India)

    2011-03-15

    {alpha}-lactose monohydrate is widely used as a pharmaceutical excipient. Drug delivery system requires the excipient to be of narrow particle size distribution with regular particle shape. Application of ultrasound is known to increase or decrease the growth rate of certain crystal faces and controls the crystal size distribution. In the present paper, effect of process parameters such as sonication time, anti-solvent concentration, initial lactose concentration and initial pH of sample on lactose crystal size, shape and thermal transition temperature was studied. The parameters were set according to the L{sub 9}-orthogonal array method at three levels and recovered lactose from whey by sonocrystallization. The recovered lactose was analyzed by particle size analyzer, scanning electron microscopy and differential scanning calorimeter. It was found that the morphology of lactose crystal was rod/needle like shape. Crystal size distribution of lactose was observed to be influenced by different process parameters. From the results of analysis of variance, the sonication time interval was found to be the most significant parameter affecting the volume median diameter of lactose with the highest percentage contribution (74.28%) among other parameters. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  16. Random photonic crystal optical memory

    International Nuclear Information System (INIS)

    Wirth Lima Jr, A; Sombra, A S B

    2012-01-01

    Currently, optical cross-connects working on wavelength division multiplexing systems are based on optical fiber delay lines buffering. We designed and analyzed a novel photonic crystal optical memory, which replaces the fiber delay lines of the current optical cross-connect buffer. Optical buffering systems based on random photonic crystal optical memory have similar behavior to the electronic buffering systems based on electronic RAM memory. In this paper, we show that OXCs working with optical buffering based on random photonic crystal optical memories provides better performance than the current optical cross-connects. (paper)

  17. Rapid X-ray crystal structure analysis in few second measurements using microstrip gas chamber

    CERN Document Server

    Ochi, A; Tanimori, T; Ohashi, Y; Toyokawa, H; Nishi, Y; Nishi, Y; Nagayoshi, T; Koishi, S

    2001-01-01

    X-ray crystal structure analysis using microstrip gas chamber was successfully carried out in a measurement time within a few seconds. The continuous rotation photograph method, in which most of the diffraction peaks can be obtained within one continuous rotation of the sample crystal (without stopping or oscillation), was applied for this measurement. As an example, the structure of a single crystal of ammonium bitartrate (r=1 mm, spherical) was measured. Diffraction spots from the sample, which were sufficient to obtain crystal structure, were successfully obtained by taking only 2 s measurements with a commercially available laboratory X-ray source.

  18. Crystal growth, spectroscopic characterization and laser performance of Tm/Mg:LiNbO3 crystal

    Science.gov (United States)

    Zhang, P. X.; Yin, J. G.; Zhang, R.; Li, H. Q.; Xu, J. Q.; Hang, Y.

    2014-03-01

    A Tm, Mg co-doped LiNbO3 crystal was grown by the traditional Czochralski method. The room-temperature absorption, photo-luminescence spectra and fluorescence lifetime of Tm3+ ions in the crystal have been investigated. The experimental results show that the co-doped of MgO can lead to the lengthening of the measured fluorescence lifetime of the upper Tm3+:3F4 level. Based on the Judd-Ofelt approach, the intensity parameters Ω2,4,6 of Tm3+ were calculated to be Ω2 (6.29 × 10-20 cm2), Ω4 (0.54 × 10-20 cm2) and Ω6 (0.79 × 10-20 cm2). Other spectroscopic parameters that relate to laser performance were also obtained. Non-photorefractive continuous wave laser operation with a Tm, Mg:LiNbO3 single crystal is demonstrated at room temperature for the first time. We obtained 1.026 W output power at 1.885 μm with a slope efficiency of near 14%, which, to the best of our knowledge, is the largest output power and the highest slope efficiency obtained for this crystal thus far. The output power was observed to be stable, and the crystal showed no sign of photorefractive damage.

  19. Unsolved problems of crystallization and melting of flexible macromolecules

    International Nuclear Information System (INIS)

    Wunderlich, B.

    1992-01-01

    The thermodynamics, kinetics, and computer simulations of crystallization and melting is discussed. The thermodynamics is shown to be well understood, although for many specific crystals not enough details for full description are available. Experiments on the crystallization kinetics of poly(ethylene) and poly(oxyethylene) in the presence of crystal nuclei as a function of molecular mass revealed that with increasing mass, the crystallization behavior deviates increasingly from that of small, rigid molecules. Instead of showing a continuously changing, linear crystallization rate with temperature through the equilibrium melting temperature, T m 0 , these flexible macromolecules show a region of practically zero crystallization rate between T m 0 and about (T m 0 - 15) K, creating a temperature region of metastability in the melt that cannot be broken by nucleation with pregrown crystals. Molecular Nucleation was proposed as a cooperative process to be of overriding importance for the description of polymer crystallization, and to be at the center of segregation of molecules of lower molecular mass by growing crystal fronts. Initial efforts to model sufficiently large crystals using Monte Carlo and molecular dynamics methods are presented. Some of the short-time intermediates in the melting, crystallization, and annealing processes seem to have little similarity to commonly assumed models of crystallization and melting and are presented as discussion topics

  20. Pressure-induced melting of micellar crystal

    DEFF Research Database (Denmark)

    Mortensen, K.; Schwahn, D.; Janssen, S.

    1993-01-01

    that pressure improves the solvent quality of water, thus resulting in decomposition of the micelles and consequent melting of the micellar crystal. The combined pressure and temperature dependence reveals that in spite of the apparent increase of order on the 100 angstrom length scale upon increasing......Aqueous solutions of triblock copolymers of poly(ethylene oxide) and poly(propylene oxide) aggregate at elevated temperatures into micelles which for polymer concentrations greater-than-or-equal-to 20% make a hard sphere crystallization to a cubic micellar crystal. Structural studies show...... temperature (decreasing pressure) the overall entropy increases through the inverted micellar crystallization characteristic....

  1. Study on the NaOH/metakaolin ratio and crystallization time for zeolite a synthesis from kaolin using statistical design

    Energy Technology Data Exchange (ETDEWEB)

    Silva Filho, Severino Higino da; Bieseki, Lindiane; Pergher, Sibele Berenice Castella, E-mail: sibelepergher@gmail.com [Universidade Federal do Rio Grande do Norte (LABPEMOL/UFRN), Natal, RN (Brazil). Lab. de Peneiras Moleculares; Maia, Ana Aurea B.; Angelica, Romulo Simoes [Universidade Federal do Para (UFPA), Belem PA (Brazil); Treichel, Helen [Universidade Federal da Fronteira Sil (UFFS), Erechim, RS (Brazil)

    2017-05-15

    The NaOH/metakaolin ratio and crystallization time were studied for the synthesis of zeolite NaA from a sample of kaolin from a Capim mine. The tests were carried out by using statistical design with axial points and replication of the central point. The samples obtained were characterized by X-ray diffraction (DRX), scanning electron microscopy and chemical analysis using a microprobe EPMA. The results showed that there is a relationship between the amount of NaOH added and crystallization time. The tests carried out using the lowest NaOH/metakaolin ratio (0.5) and the shortest time (4 h) produced a non-crystalline material. On the other hand, increasing the NaOH/metakaolin ratio and the crystallization time led to the formation of a NaA phase with a high structural level, but with the presence of a sodalite phase as an impurity. (author)

  2. Glass formation and crystallization of Zr53Cu21Al10Ni8Ti8 alloy

    International Nuclear Information System (INIS)

    Neogy, S.; Tewari, R.; Srivastava, D.; Dey, G.K.; Banerjee, S.; Vaibhaw, K.; Ranganathan, S.

    2010-01-01

    In the present study, transmission electron microscopy techniques, like micro-diffraction, high resolution and fluctuation microscopy, have been employed to carry out detailed investigation of as-solidified and crystallized microstructures of the Zr 53 Cu 21 Al 10 Ni 8 Ti 8 alloy synthesized using melt spinning, suction casting and copper mould casting techniques. Samples produced by copper mould casting technique showed partially crystalline microstructure whereas the other techniques resulted in complete amorphous microstructures. High-resolution microscopy established that the dendrites of the big cube phase in partially crystalline glass grew by atomistic ledges. The other crystalline bct Zr 2 Ni phase, present in partially crystalline glass and also in all the crystallized microstructures, showed various types of internal faults depending upon the crystallite size. Fluctuation microscopy established that oxygen plays a major role in determining the degree of medium range order in glassy phases. In addition, variation in oxygen content changed the crystallization behaviour of glasses from a single to multiple events

  3. Growth and optical studies of opal films as three-dimensional photonic crystals

    Energy Technology Data Exchange (ETDEWEB)

    Comoretto, D.; Grassi, R.; Marabelli, F.; Andreani, L.C

    2003-01-15

    Three-dimensional artificial opals showing photonic crystals properties are grown by self-assembly of polystyrene nanospheres. Atomic force microscopy (AFM) images of opal surfaces show domains with regular triangular and squared packing of the spheres separated by cracks whose relative fraction depends on the sample quality. The energy position of an optical pseudo gap in transmittance spectra is observed by varying the angle of incidence and is accounted for by theoretical calculations of the photonic band structure based on a plane-wave expansion method.

  4. Growth and optical studies of opal films as three-dimensional photonic crystals

    International Nuclear Information System (INIS)

    Comoretto, D.; Grassi, R.; Marabelli, F.; Andreani, L.C.

    2003-01-01

    Three-dimensional artificial opals showing photonic crystals properties are grown by self-assembly of polystyrene nanospheres. Atomic force microscopy (AFM) images of opal surfaces show domains with regular triangular and squared packing of the spheres separated by cracks whose relative fraction depends on the sample quality. The energy position of an optical pseudo gap in transmittance spectra is observed by varying the angle of incidence and is accounted for by theoretical calculations of the photonic band structure based on a plane-wave expansion method

  5. Quartz Crystal Temperature Sensor for MAS NMR

    Science.gov (United States)

    Simon, Gerald

    1997-10-01

    Quartz crystal temperature sensors (QCTS) were tested for the first time as wireless thermometers in NMR MAS rotors utilizing the NMR RF technique itself for exiting and receiving electro-mechanical quartz resonances. This new tool in MAS NMR has a high sensitivity, linearity, and precision. When compared to the frequently used calibration of the variable temperature in the NMR system by a solid state NMR chemical shift thermometer (CST), such as lead nitrate, QCTS shows a number of advantages. It is an inert thermometer in close contact with solid samples operating parallel to the NMR experiment. QCTS can be manufactured for any frequency to be near a NMR frequency of interest (typically 1 to 2 MHz below or above). Due to the strong response of the crystal, signal detection is possible without changing the tuning of the MAS probe. The NMR signal is not influenced due to the relative sharp crystal resonance, restricted excitation by finite pulses, high probeQvalues, and commonly used audio filters. The quadratic dependence of the temperature increase on spinning speed is the same for the QCTS and for the CST lead nitrate and is discussed in terms of frictional heat in accordance with the literature about lead nitrate and with the results of a simple rotor speed jump experiment with differently radial located lead nitrate in the rotor.

  6. CH3NH3PbCl3 Single Crystals: Inverse Temperature Crystallization and Visible-Blind UV-Photodetector

    KAUST Repository

    Maculan, Giacomo; Sheikh, Arif D.; Abdelhady, Ahmed L.; Saidaminov, Makhsud I.; Haque, Mohammed; Banavoth, Murali; Alarousu, Erkki; Mohammed, Omar F.; Wu, Tao; Bakr, Osman

    2015-01-01

    a new method of sizeable CH3NH3PbCl3 single crystal growth based on retrograde solubility behavior of hybrid perovskites. We show, for the first time, the energy band structure, charge-carrier recombination and transport properties of single crystal

  7. The modification of LiTaO3 crystal by low-energy He-ion implantation

    International Nuclear Information System (INIS)

    Pang, L.L.; Wang, Z.G.; Jin, Y.F.; Yao, C.F.; Cui, M.H.; Sun, J.R.; Shen, T.L.; Wei, K.F.; Zhu, Y.B.; Sheng, Y.B.; Li, Y.F.

    2012-01-01

    Highlights: ► LiTaO 3 crystal was implanted by 250 keV He + . ► We report the surface and transmittance of LiTaO 3 change with the fluence and time. ► New phenomena (self-splitting, self-exfoliation, self-recovery) occurred. ► Evolvement of defects and the behavior of helium were discussed. - Abstract: The effects of He-ion implantation on the surface morphology and transmittance of LiTaO 3 single crystals are investigated. The samples were implanted with 250 keV He-ion at different fluences at room temperature. The results show that the surface morphology and transmittance of implanted samples strongly depend on the ion fluence and the time when the samples expose to the air up to 60 days. When the fluence is above 1.0 × 10 16 He + /cm 2 , the transmission spectra indicate that a high concentration of defects is created. 3D-profile images show that at the higher fluence a great many triangular stripes appear on the surface of the samples. After 60 days, the recovery of the transmittance occurs and varies with the fluence. For the sample at the fluence of 5.0 × 10 16 He + /cm 2 , the raised stripes on the surface evolve into narrow cracks. Regional exfoliation, however, occurs on the surface of the sample with the fluence of 1.0 × 10 17 He + /cm 2 . According to the experimental results and simulation of SRIM 2008 code, the evolvement of defects and the behavior of He are discussed.

  8. Competitive crystallization of a propylene/ethylene random copolymer filled with a β-nucleating agent and multi-walled carbon nanotubes. Conventional and ultrafast DSC study.

    Science.gov (United States)

    Papageorgiou, Dimitrios G; Papageorgiou, George Z; Zhuravlev, Evgeny; Bikiaris, Dimitrios; Schick, Christoph; Chrissafis, Konstantinos

    2013-11-27

    A propylene/ethylene polymeric matrix was reinforced by the simultaneous addition of a β-nucleating agent (calcium pimelate) and multi-walled carbon nanotubes (MWCNTs) in various concentrations. The present manuscript explores the competitive crystallization tendency that is caused by the presence of the two fillers. On the one hand, calcium pimelate forces the material to crystallize predominantly in the β-crystalline form, while, on the other, the strong α-nucleating ability of MWCNTs compels the material to develop higher α-crystalline content. An in-depth study has been performed on the nanocomposite samples by means of conventional, temperature-modulated, and differential fast scanning calorimetry (DFSC) under various dynamic and isothermal conditions. The results showed that β-crystals are predominant at low MWCNT content (DSC, and the use of very high cooling rates by UFDSC made it possible to achieve and study the nucleation of the samples. The presence of MWCNTs enabled the nanocomposites to crystallize faster under both isothermal and dynamic conditions. The activation energy of the samples was also calculated according to Friedman's theory.

  9. Single crystal growth and characterization of kagomé-lattice shandites Co3Sn2-xInxS2

    Science.gov (United States)

    Kassem, Mohamed A.; Tabata, Yoshikazu; Waki, Takeshi; Nakamura, Hiroyuki

    2015-09-01

    Single crystals of the shandite-type half metallic ferromagnet Co3Sn2S2, and its In-substituted compounds, Co3Sn2-xInxS2 (0crystals. Single crystals of the two end members, Co3Sn2S2 and Co3In2S2, and solid solutions with low In concentrations (x≤0.35) were grown out of Sn and In self flux. Solid solution single crystals with higher In concentrations were grown out of Sn, In and Pb mixture flux. Grown crystals were characterized using the powder x-ray diffraction, wavelength-dispersive x-ray spectroscopy and magnetization measurements. The shandite structure with R3¯m symmetry was confirmed and crystal structure parameters of the obtained plate-shaped hexagonal crystals were refined using the Rietveld analysis. Magnetization measurements show suppression of the ferromagnetic ordering, observed in Co3Sn2S2, by In-substitution as reported for polycrystalline samples. The obtained crystals are useful to study anisotropy in magnetic and transport properties and further interesting magnetotransport properties of the layered compounds.

  10. Unidirectional Wave Propagation in Low-Symmetric Colloidal Photonic-Crystal Heterostructures

    OpenAIRE

    Yannopapas, Vassilios

    2015-01-01

    We show theoretically that photonic crystals consisting of colloidal spheres exhibit unidirectional wave propagation and one-way frequency band gaps without breaking time-reversal symmetry via, e.g., the application of an external magnetic field or the use of nonlinear materials. Namely, photonic crystals with low symmetry such as the monoclinic crystal type considered here as well as with unit cells formed by the heterostructure of different photonic crystals show significant unidirectional ...

  11. [Features of calcium crystals and calcium components in 54 plant species in salinized habitats of Tianjin].

    Science.gov (United States)

    Xu, Jing-Jing; Ci, Hua-Cong; He, Xing-Dong; Xue, Ping-Ping; Zhao, Xue-Lai; Guo, Jian-Tan; Gao, Yu-Bao

    2012-05-01

    Plant calcium (Ca) is composed of dissociated Ca2+ and easily soluble, slightly soluble, and hard soluble combined Ca salts. The hard soluble Ca salts can often engender Ca crystals. To understand the Ca status in different growth form plants in salinized habitats, 54 plant species were sampled from the salinized habitats in Tianjin, with the Ca crystals examined by microscope and the Ca components determined by sequential fractionation procedure. More Ca crystals were found in 38 of the 54 plant species. In 37 of the 38 plant species, drusy and prismatic Ca oxalate crystals dominated, whereas the cystolith of Ca carbonate crystal only appeared in the leaves of Ficus carica of Moraceae. The statistics according to growth form suggested that deciduous arbors and shrubs had more Ca oxalate crystal, liana had lesser Ca oxalate crystal, and herbs and evergreen arbors had no Ca oxalate crystal. From arbor, shrub, liana to herb, the concentration of HCl-soluble Ca decreased gradually, while that of water soluble Ca was in adverse. The concentration of water soluble Ca in herbs was significantly higher than that in arbors and shrubs. This study showed that in salinized habitats, plant Ca crystals and Ca components differed with plant growth form, and the Ca oxalate in deciduous arbors and shrubs played an important role in withstanding salt stress.

  12. Solid state structural investigations of the bis(chalcone) compound with single crystal X-ray crystallography, DFT, gamma-ray spectroscopy and chemical spectroscopy methods

    Science.gov (United States)

    Yakalı, Gül; Biçer, Abdullah; Eke, Canel; Cin, Günseli Turgut

    2018-04-01

    A bis(chalcone), (2E,6E)-2,6-bis((E)-3phenylallidene)cyclohexanone, was characterized by 1H NMR, 13C NMR, FTIR, UV-Vis spectroscopy, gamma-ray spectroscopy and single crystal X- ray structural analysis. The optimized molecular structure of the compound is calculated using DFT/B3LYP with 6-31G (d,p) level. The calculated geometrical parameters are in good agreement with the experimental data obtained from our reported X-ray structure. The powder and single crystal compounds were gama-irradiated using clinical electron linear accelerator and 60Co gamma-ray source, respectively. Spectral studies (1H NMR, 13C NMR, FTIR and UV-Vis) of powder chalcone compound were also investigated before and after irradiation. Depending on the irradiation notable changes were observed in spectral features powder sample. Single crystal X-ray diffraction investigation shows that both unirradiated and irradiated single crystal samples crystallizes in a orthorhombic crystal system in the centrosymmetric space group Pbcn and exhibits an C-H..O intramolecular and intermolecular hydrogen bonds. The crystal packing is stabilised by strong intermolecular bifurcate C-H..O hydrogen bonds and π…π stacking interactions. The asymmetric unit of the title compound contains one-half of a molecule. The other half of the molecule is generated with (1-x,y,-3/2-z) symmetry operator. The molecule is almost planar due to having π conjugated system of chalcones. However, irradiated single crystal compound showed significant changes lattice parameters, crystal volume and density. According to results of gamma-ray spectroscopy, radioactive elements of powder compound which are 123Sb(n,g),124Sb,57Fe(g,p),56Mn, 55Mn(g,n), and 54Mn were determined using photoactivation analysis. However, the most intensive gamma-ray energy signals are 124Sb.

  13. Fluid Physics and Macromolecular Crystal Growth in Microgravity

    Science.gov (United States)

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

    2000-01-01

    The first protein crystallization experiment in microgravity was launched in April, 1981 and used Germany's Technologische Experimente unter Schwerelosigkeit (TEXUS 3) sounding rocket. The protein P-galactosidase (molecular weight 465Kda) was chosen as the sample with a liquid-liquid diffusion growth method. A sliding device brought the protein, buffer and salt solution into contact when microgravity was reached. The sounding rocket gave six minutes of microgravity time with a cine camera and schlieren optics used to monitor the experiment, a single growth cell. In microgravity a strictly laminar diffusion process was observed in contrast to the turbulent convection seen on the ground. Several single crystals, approx 100micron in length, were formed in the flight which were of inferior but of comparable visual quality to those grown on the ground over several days. A second experiment using the same protocol but with solutions cooled to -8C (kept liquid with glycerol antifreeze) again showed laminar diffusion. The science of macromolecular structural crystallography involves crystallization of the macromolecule followed by use of the crystal for X-ray diffraction experiments to determine the three dimensional structure of the macromolecule. Neutron protein crystallography is employed for elucidation of H/D exchange and for improved definition of the bound solvent (D20). The structural information enables an understanding of how the molecule functions with important potential for rational drug design, improved efficiency of industrial enzymes and agricultural chemical development. The removal of turbulent convection and sedimentation in microgravity, and the assumption that higher quality crystals will be produced, has given rise to the growing number of crystallization experiments now flown. Many experiments can be flown in a small volume with simple, largely automated, equipment - an ideal combination for a microgravity experiment. The term "protein crystal growth

  14. Lithium niobate bulk crystallization promoted by CO2 laser radiation

    Science.gov (United States)

    Ferreira, N. M.; Costa, F. M.; Nogueira, R. N.; Graça, M. P. F.

    2012-09-01

    The crystallization induced by laser radiation is a very promising technique to promote glass/ceramic transformation, being already used to produce crystalline patterns on glass surfaces. In this work, a SiO2-Li2O-Nb2O5 glass, prepared by the sol-gel route, was submitted to CO2 laser radiation and conventional heat-treatments in order to induce the LiNbO3 crystallization. The structure and morphology of the samples prepared by both routes was analyzed as a function of exposure time, radiation power and heat-treatment temperatures by XRD, Raman spectroscopy and SEM. The results reveal a correlation between the crystallization degree of LiNbO3 particles and glass matrix with the heat treatment type and experimental parameters. An heat-treatment at 650 °C/4 h was necessary to induce crystallization in heat treatments samples while 4 W/500 s was enough for laser radiation ones, corresponding a reduction time processing of ˜14 000 s.

  15. Influence of Substrate on Crystal Orientation of Large-Grained Si Thin Films Formed by Metal-Induced Crystallization

    Directory of Open Access Journals (Sweden)

    Kaoru Toko

    2015-01-01

    Full Text Available Producing large-grained polycrystalline Si (poly-Si film on glass substrates coated with conducting layers is essential for fabricating Si thin-film solar cells with high efficiency and low cost. We investigated how the choice of conducting underlayer affected the poly-Si layer formed on it by low-temperature (500°C Al-induced crystallization (AIC. The crystal orientation of the resulting poly-Si layer strongly depended on the underlayer material: (100 was preferred for Al-doped-ZnO (AZO and indium-tin-oxide (ITO; (111 was preferred for TiN. This result suggests Si heterogeneously nucleated on the underlayer. The average grain size of the poly-Si layer reached nearly 20 µm for the AZO and ITO samples and no less than 60 µm for the TiN sample. Thus, properly electing the underlayer material is essential in AIC and allows large-grained Si films to be formed at low temperatures with a set crystal orientation. These highly oriented Si layers with large grains appear promising for use as seed layers for Si light-absorption layers as well as for advanced functional materials.

  16. Shear induced structures in crystallizing cocoa butter

    Science.gov (United States)

    Mazzanti, Gianfranco; Guthrie, Sarah E.; Sirota, Eric B.; Marangoni, Alejandro G.; Idziak, Stefan H. J.

    2004-03-01

    Cocoa butter is the main structural component of chocolate and many cosmetics. It crystallizes in several polymorphs, called phases I to VI. We used Synchrotron X-ray diffraction to study the effect of shear on its crystallization. A previously unreported phase (phase X) was found and a crystallization path through phase IV under shear was observed. Samples were crystallized under shear from the melt in temperature controlled Couette cells, at final crystallization temperatures of 17.5^oC, 20^oC and 22.5^oC in Beamline X10A of NSLS. The formation of phase X was observed at low shear rates (90 s-1) and low crystallization temperature (17.5^oC), but was absent at high shear (720 s-1) and high temperature (20^oC). The d-spacing and melting point suggest that this new phase is a mixture rich on two of the three major components of cocoa butter. We also found that, contrary to previous reports, the transition from phase II to phase V can happen through the intermediate phase IV, at high shear rates and temperature.

  17. Versatile Collimating Crystal Stage for a Bonse-Hart USAXS Instrument

    International Nuclear Information System (INIS)

    Ilavsky, J.; Shu, D.; Jemian, P. R.; Long, G. G.

    2007-01-01

    An advanced ultra-small-angle X-ray scattering (USAXS) instrument, using the Bonse-Hart design and installed at APS, is a robust and reliable instrument, providing a scattering vector (q) range of nearly 4 decades (0.00015 to 1 Aa-1), an intensity dynamic range of up to 9 decades, standard-less absolute intensity calibration, and USAXS imaging capabilities. This type of instrument typically uses channel-cut crystals in both the collimating (before sample) and analyzing (after sample) stages. The optical surfaces of these crystals are finished by etching processes, which leave an orange-peel surface texture, which would compromise the USAXS imaging quality. Therefore optics with highly polished surfaces using separated crystals in both collimating and analyzing stages were developed. A novel design of the optics and mechanical stage uses a fixed gap between the two separated collimating crystals in which a triangular section of the first crystal is removed, allowing for a variable number (1, 2, 4, 6, or 8) of crystal reflections for X-ray energies between 7 and 19 keV. The number of reflections is selected by lateral translation of the collimating crystal pair. Rotational alignment of the second crystal in the pair by an artificial channel-cut crystal mechanism, implemented with a novel high-stiffness weak link actuated by both a picomotor and a piezo-electric transducer, provides the capability to align or adjust an assembly of crystals to achieve the same performance as a single channel-cut crystal with integral weak link. The arrangement of both crystals is held on a removable base that can be remounted with precision within the Si(111) rocking curve on a three-point kinematic mount. Additional tilt adjustments are also provided for initial alignment. This monochromator has proven to be highly robust with respect to motions and vibrations, as well as flexible with respect to selection of number of reflections, and its performance directly resulted in the highly

  18. A novel storage system for cryoEM samples.

    Science.gov (United States)

    Scapin, Giovanna; Prosise, Winifred W; Wismer, Michael K; Strickland, Corey

    2017-07-01

    We present here a new CryoEM grid boxes storage system designed to simplify sample labeling, tracking and retrieval. The system is based on the crystal pucks widely used by the X-ray crystallographic community for storage and shipping of crystals. This system is suitable for any cryoEM laboratory, but especially for large facilities that will need accurate tracking of large numbers of samples coming from different sources. Copyright © 2017. Published by Elsevier Inc.

  19. Draft Tube Baffle (DTB) crystallizers: A study of stationary and dynamically behaving Crystal Size Distributions (CSD)

    Science.gov (United States)

    Deleer, B. G. M.

    1981-11-01

    Based on population balance, CSD behavior as a function of geometrical and operating variables was studied, using a crystallizer. A potash alum-water system, involving a separation technique which uses surface active agents and an apolar, organic liquid to separate potash alum crystals from mother liquid under the influence of gravity was used to check experimental findings against literature data. Results show action of annular settling spaces is strongly influenced by fluid velocities perpendicular to those directed upwards. The well-mixed volume decreases with increasing crystallizer size until a minimum effective volume is reached. As supersaturation is constant throughout the crystallizer volume under stationary operating conditions, the annular settling space behaves like a growth chamber for crystals in its volume. Swirl in the lower part of the annular volume introduces significant back mixing. Crystals within this space either grow and return to the well-mixed part, or withdraw from the annular volume permanently.

  20. Development of an X-ray fluorescence holographic measurement system for protein crystals

    International Nuclear Information System (INIS)

    Sato-Tomita, Ayana; Shibayama, Naoya; Okabe, Takahiro; Happo, Naohisa; Kimura, Koji; Matsushita, Tomohiro; Park, Sam-Yong; Sasaki, Yuji C.; Hayashi, Kouichi

    2016-01-01

    Experimental procedure and setup for obtaining X-ray fluorescence hologram of crystalline metalloprotein samples are described. Human hemoglobin, an α_2β_2 tetrameric metalloprotein containing the Fe(II) heme active-site in each chain, was chosen for this study because of its wealth of crystallographic data. A cold gas flow system was introduced to reduce X-ray radiation damage of protein crystals that are usually fragile and susceptible to damage. A χ-stage was installed to rotate the sample while avoiding intersection between the X-ray beam and the sample loop or holder, which is needed for supporting fragile protein crystals. Huge hemoglobin crystals (with a maximum size of 8 × 6 × 3 mm"3) were prepared and used to keep the footprint of the incident X-ray beam smaller than the sample size during the entire course of the measurement with the incident angle of 0°-70°. Under these experimental and data acquisition conditions, we achieved the first observation of the X-ray fluorescence hologram pattern from the protein crystals with minimal radiation damage, opening up a new and potential method for investigating the stereochemistry of the metal active-sites in biomacromolecules.

  1. Liquid crystal-based Mueller matrix spectral imaging polarimetry for parameterizing mineral structural organization.

    Science.gov (United States)

    Gladish, James C; Duncan, Donald D

    2017-01-20

    Herein, we discuss the remote assessment of the subwavelength organizational structure of a medium. Specifically, we use spectral imaging polarimetry, as the vector nature of polarized light enables it to interact with optical anisotropies within a medium, while the spectral aspect of polarization is sensitive to small-scale structure. The ability to image these effects allows for inference of spatial structural organization parameters. This work describes a methodology for revealing structural organization by exploiting the Stokes/Mueller formalism and by utilizing measurements from a spectral imaging polarimeter constructed from liquid crystal variable retarders and a liquid crystal tunable filter. We provide results to validate the system and then show results from measurements on a mineral sample.

  2. Impact of Heterogeneity and Lattice Bond Strength on DNA Triangle Crystal Growth.

    Science.gov (United States)

    Stahl, Evi; Praetorius, Florian; de Oliveira Mann, Carina C; Hopfner, Karl-Peter; Dietz, Hendrik

    2016-09-07

    One key goal of DNA nanotechnology is the bottom-up construction of macroscopic crystalline materials. Beyond applications in fields such as photonics or plasmonics, DNA-based crystal matrices could possibly facilitate the diffraction-based structural analysis of guest molecules. Seeman and co-workers reported in 2009 the first designed crystal matrices based on a 38 kDa DNA triangle that was composed of seven chains. The crystal lattice was stabilized, unprecedentedly, by Watson-Crick base pairing. However, 3D crystallization of larger designed DNA objects that include more chains such as DNA origami remains an unsolved problem. Larger objects would offer more degrees of freedom and design options with respect to tailoring lattice geometry and for positioning other objects within a crystal lattice. The greater rigidity of multilayer DNA origami could also positively influence the diffractive properties of crystals composed of such particles. Here, we rationally explore the role of heterogeneity and Watson-Crick interaction strengths in crystal growth using 40 variants of the original DNA triangle as model multichain objects. Crystal growth of the triangle was remarkably robust despite massive chemical, geometrical, and thermodynamical sample heterogeneity that we introduced, but the crystal growth sensitively depended on the sequences of base pairs next to the Watson-Crick sticky ends of the triangle. Our results point to weak lattice interactions and high concentrations as decisive factors for achieving productive crystallization, while sample heterogeneity and impurities played a minor role.

  3. Bloch walls in a nickel single crystal

    International Nuclear Information System (INIS)

    Peters, J.; Treimer, W.

    2001-01-01

    We present a consistent theory for the dependence of the magnetic structure in bulk samples on external static magnetic fields and corresponding experimental results. We applied the theory of micromagnetism to this crystal and calculated the Bloch wall thickness as a function of external magnetic fields. The theoretical results agree well with the experimental data, so that the Bloch wall thickness of a 71 deg. nickel single crystal was definitely determined with some hundred of nanometer

  4. Non-isothermal crystallization kinetics and characterization of biodegradable poly(butylene succinate-co-neopentyl glycol succinate) copolyesters.

    Science.gov (United States)

    Xie, Wen-Jie; Zhou, Xiao-Ming

    2015-01-01

    Both biodegradable aliphatic neat poly(butylene succinate) (PBS) and poly(butylene succinate-co-neopentyl glycol succinate) (P(BS-co-NPGS)) copolyesters with different 1,4-butanediol/neopentyl glycol ratios were synthesized through a two-step process of transesterification and polycondensation using stannous chloride and 4-Methylbenzenesulfonic acid as the co-catalysts. The structure, non-isothermal crystallization behavior, crystalline morphology and crystal structure of neat PBS and P(BS-co-NPGS) copolyesters were characterized by (1)H NMR, differential scanning calorimetry (DSC), polarized optical microscope (POM) and wide angle X-ray diffraction (WAXD), respectively. The Avrami equation modified by Jeziorny and Mo's method was employed to describe the non-isothermal crystallization kinetics of the neat PBS and its copolyesters. The modified Avrami equation could adequately describe the primary stage of non-isothermal crystallization kinetics of the neat PBS and its copolyesters. Mo's method provided a fairly satisfactory description of the non-isothermal crystallization of neat PBS and its copolyesters. Interestingly, the values of 1/t1/2, Zc and F(T) obtained by the modified Avrami equation and Mo's method analysis indicated that the crystallization rate increased first and then decreased with an increase of NPGS content compared that of neat PBS, whereas the crystallization mechanism almost kept unchanged. The results of tensile testing showed that the ductility of PBS was largely improved by incorporating NPGS units. The elongation at break increased remarkably with increasing NPGS content. In particular, the sample with 20% NPGS content showed around 548% elongation at break. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Effects of high-dose hydrogen implantation on defect formation and dopant diffusion in silver implanted ZnO crystals

    Energy Technology Data Exchange (ETDEWEB)

    Yaqoob, Faisal [Department of Physics, State University of New York at Albany, Albany, New York 12222 (United States); Huang, Mengbing, E-mail: mhuang@sunypoly.edu [College of Nanoscale Science and Engineering, State University of New York Polytechnic Institute, Albany, New York 12203 (United States)

    2016-07-28

    This work reports on the effects of a deep high-dose hydrogen ion implant on damage accumulation, defect retention, and silver diffusion in silver implanted ZnO crystals. Single-crystal ZnO samples were implanted with Ag ions in a region ∼150 nm within the surface, and some of these samples were additionally implanted with hydrogen ions to a dose of 2 × 10{sup 16 }cm{sup −2}, close to the depth ∼250 nm. Rutherford backscattering/ion channeling measurements show that crystal damage caused by Ag ion implantation and the amount of defects retained in the near surface region following post-implantation annealing were found to diminish in the case with the H implantation. On the other hand, the additional H ion implantation resulted in a reduction of substitutional Ag atoms upon post-implantation annealing. Furthermore, the presence of H also modified the diffusion properties of Ag atoms in ZnO. We discuss these findings in the context of the effects of nano-cavities on formation and annihilation of point defects as well as on impurity diffusion and trapping in ZnO crystals.

  6. Crystallization and preliminary X-ray structural studies of hemoglobin A2 and hemoglobin E, isolated from the blood samples of β-thalassemic patients

    International Nuclear Information System (INIS)

    Dasgupta, Jhimli; Sen, Udayaditya; Choudhury, Debi; Datta, Poppy; Chakrabarti, Abhijit; Chakrabarty, Sudipa Basu; Chakrabarty, Amit; Dattagupta, J.K.

    2003-01-01

    Hemoglobin A 2 (α 2 δ 2 ), a minor (2-3%) component of circulating red blood cells, acts as an anti-sickling agent and its elevated concentration in β-thalassemia is a useful clinical diagnostic. In β-thalassemia major, where there is a failure of β-chain production, HbA 2 acts as the predominant oxygen deliverer. Hemoglobin E, is another common abnormal hemoglobin, caused by splice site mutation in exon 1 of β globin gene, when combines with β-thalassemia, causes severe microcytic anemia. The purification, crystallization, and preliminary structural studies of HbA 2 and HbE are reported here. HbA 2 and HbE are purified by cation exchange column chromatography in presence of KCN from the blood samples of individuals suffering from β-thalassemia minor and Eβ-thalassemia. X-ray diffraction data of HbA 2 and HbE were collected upto 2.1 and 1.73 A, respectively. HbA 2 crystallized in space group P2 1 with unit cell parameters a=54.33 A, b=83.73 A, c=62.87 A, and β=99.80 degree sign whereas HbE crystallized in space group P2 1 2 1 2 1 with unit cell parameters a=60.89 A, b=95.81 A, and c=99.08 A. Asymmetric unit in each case contains one Hb tetramer in R 2 state

  7. Potassium acceptor doping of ZnO crystals

    Directory of Open Access Journals (Sweden)

    Narendra S. Parmar

    2015-05-01

    Full Text Available ZnO bulk single crystals were doped with potassium by diffusion at 950°C. Positron annihilation spectroscopy confirms the filling of zinc vacancies and a different trapping center for positrons. Secondary ion mass spectroscopy measurements show the diffusion of potassium up to 10 μm with concentration ∼1 × 1016 cm−3. IR measurements show a local vibrational mode (LVM at 3226 cm−1, at a temperature of 9 K, in a potassium doped sample that was subsequently hydrogenated. The LVM is attributed to an O–H bond-stretching mode adjacent to a potassium acceptor. When deuterium substitutes for hydrogen, a peak is observed at 2378 cm−1. The O-H peak is much broader than the O-D peak, perhaps due to an unusually low vibrational lifetime. The isotopic frequency ratio is similar to values found in other hydrogen complexes. Potassium doping increases the resistivity up to 3 orders of magnitude at room temperature. The doped sample has a donor level at 0.30 eV.

  8. Potassium acceptor doping of ZnO crystals

    Science.gov (United States)

    Parmar, Narendra S.; Corolewski, Caleb D.; McCluskey, Matthew D.; Lynn, K. G.

    2015-05-01

    ZnO bulk single crystals were doped with potassium by diffusion at 950°C. Positron annihilation spectroscopy confirms the filling of zinc vacancies and a different trapping center for positrons. Secondary ion mass spectroscopy measurements show the diffusion of potassium up to 10 μm with concentration ˜1 × 1016 cm-3. IR measurements show a local vibrational mode (LVM) at 3226 cm-1, at a temperature of 9 K, in a potassium doped sample that was subsequently hydrogenated. The LVM is attributed to an O-H bond-stretching mode adjacent to a potassium acceptor. When deuterium substitutes for hydrogen, a peak is observed at 2378 cm-1. The O-H peak is much broader than the O-D peak, perhaps due to an unusually low vibrational lifetime. The isotopic frequency ratio is similar to values found in other hydrogen complexes. Potassium doping increases the resistivity up to 3 orders of magnitude at room temperature. The doped sample has a donor level at 0.30 eV.

  9. Potassium acceptor doping of ZnO crystals

    Energy Technology Data Exchange (ETDEWEB)

    Parmar, Narendra S., E-mail: nparmar@wsu.edu; Lynn, K. G. [Center for Materials Research, Washington State University, Pullman, Washington 99164-2711 (United States); Department of Physics and Astronomy, Washington State University, Pullman, Washington 99164-2814 (United States); Corolewski, Caleb D.; McCluskey, Matthew D. [Department of Physics and Astronomy, Washington State University, Pullman, Washington 99164-2814 (United States)

    2015-05-15

    ZnO bulk single crystals were doped with potassium by diffusion at 950°C. Positron annihilation spectroscopy confirms the filling of zinc vacancies and a different trapping center for positrons. Secondary ion mass spectroscopy measurements show the diffusion of potassium up to 10 μm with concentration ∼1 × 10{sup 16} cm{sup −3}. IR measurements show a local vibrational mode (LVM) at 3226 cm{sup −1}, at a temperature of 9 K, in a potassium doped sample that was subsequently hydrogenated. The LVM is attributed to an O–H bond-stretching mode adjacent to a potassium acceptor. When deuterium substitutes for hydrogen, a peak is observed at 2378 cm{sup −1}. The O-H peak is much broader than the O-D peak, perhaps due to an unusually low vibrational lifetime. The isotopic frequency ratio is similar to values found in other hydrogen complexes. Potassium doping increases the resistivity up to 3 orders of magnitude at room temperature. The doped sample has a donor level at 0.30 eV.

  10. Electronic transport properties of single crystal thallium-2201 superconductors

    International Nuclear Information System (INIS)

    Yandrofski, R.M.

    1992-01-01

    Four-probe resistance measurements on single crystals of the calcium-free thallium-based superconducting Tl 2 Ba 2 CuO 6+σ phase (Tl-2201) were performed in magnetic fields up to 12 Telsa. Single crystals of sizes were grown by a self-flux technique and were characterized by single crystal X-ray diffraction and X-ray Dispersive Analysis. Field measurements were taken at dc and at low frequencies using a lock-in technique. Techniques were developed to oxygen-anneal the as-grown single crystals to generate single crystal samples of the same Tl-2201 phase with varying transition interaction effect against appropriate composite general alternatives are developed for the standard two-way layout with a single observation per cell. Nonparametric aligned-rank test procedures are introduced. One of the new procedures is shown to be equivalent to a slight modification of the previously studied Latin square procedures when the factors have the same number of levels. The equal in distribution technique is used to show that any statistic based on the joint ranks should not be used to test the hypotheses of interest. The tests based on aligning with the averages do not depend on the nuisance main effects, while those based on aligning with the median do depend on the nuisance main effects. The relative power performance of the competing tests are examined via Monte Carlo simulation. Power studies conducted on the 5 x 5, 5 x 6, and 5 x 9 two-way layouts with one observation per cell show that the new procedures based on a comparison of all possible pairs of rank-profiles perform quite well for two types of product interaction, a general class of interaction effects proposed by Martin, and several sets of specific interaction effects. Approximate critical values for some of the proposed procedures are explored in the special case when the main effect parameters for one factor are known

  11. Unifying the crystallization behavior of hexagonal and square crystals with the phase-field-crystal model

    International Nuclear Information System (INIS)

    Yang Tao; Chen Zheng; Zhang Jing; Wang Yongxin; Lu Yanli

    2016-01-01

    By employing the phase-field-crystal models, the atomic crystallization process of hexagonal and square crystals is investigated with the emphasis on the growth mechanism and morphological change. A unified regime describing the crystallization behavior of both crystals is obtained with the thermodynamic driving force varying. By increasing the driving force, both crystals (in the steady-state) transform from a faceted polygon to an apex-bulged polygon, and then into a symmetric dendrite. For the faceted polygon, the interface advances by a layer-by-layer (LL) mode while for the apex-bulged polygonal and the dendritic crystals, it first adopts the LL mode and then transits into the multi-layer (ML) mode in the later stage. In particular, a shift of the nucleation sites from the face center to the area around the crystal tips is detected in the early growth stage of both crystals and is rationalized in terms of the relation between the crystal size and the driving force distribution. Finally, a parameter characterizing the complex shape change of square crystal is introduced. (paper)

  12. Rapid localized crystallization of lysozyme by laser trapping.

    Science.gov (United States)

    Yuyama, Ken-Ichi; Chang, Kai-Di; Tu, Jing-Ru; Masuhara, Hiroshi; Sugiyama, Teruki

    2018-02-28

    Confining protein crystallization to a millimetre size was achieved within 0.5 h after stopping 1 h intense trapping laser irradiation, which shows excellent performance in spatial and temporal controllability compared to spontaneous nucleation. A continuous-wave near-infrared laser beam is tightly focused into a glass/solution interfacial layer of a supersaturated buffer solution of hen egg-white lysozyme (HEWL). The crystallization is not observed during laser trapping, but initiated by stopping the laser irradiation. The generated crystals are localized densely in a circular area with a diameter of a few millimetres around the focal spot and show specific directions of the optical axes of the HEWL crystals. To interpret this unique crystallization, we propose a mechanism that nucleation and the subsequent growth take place in a highly concentrated domain consisting of HEWL liquid-like clusters after turning off laser trapping.

  13. An FPGA-based slowcontrol module and a baseline shifting extension card for the sampling-ADC readout of the crystal barrel calorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Urff, Georg; Poller, Timo [Helmholtz-Institut fuer Strahlen- und Kernphysik, Bonn (Germany); Collaboration: CBELSA/TAPS-Collaboration

    2016-07-01

    At the electron accelerator ELSA (Bonn) the CBELSA/TAPS experiment investigates the photoproduction of mesons off protons and neutrons. The CsI(Tl)-crystals of the Crystal Barrel calorimeter are being upgraded from a PIN-diode readout to an APD readout. In the context of this upgrade, an FPGA-based Sampling-ADC (SADC) is presently being developed (HK 304). A Slow-control Module for the SADC with TCP/Telnet access has been developed on the basis of a Spartan6 FPGA. Control and monitoring of the SADC's power supply as well as control of parameters of the analog and digital data processing in the SADC is realized via PMBus/I{sup 2}C. The prototype as well as an overview of its functionality will be presented. In order to fully utilize the dynamic input range of the SADCs, an interfacing extension board was designed. It receives the differential signal generated by previous amplification stages and adds an individual DC offset voltage to each channel supplied by a digital-to-analog converter. The circuit and the used techniques as well as simulations and measurements are presented.

  14. The sorption of silver by poorly crystallized manganese oxides

    Science.gov (United States)

    Anderson, B.J.; Jenne, E.A.; Chao, T.T.

    1973-01-01

    The sorption of silver by poorly crystallized manganese oxides was studied using synthesized samples of three members of the manganous manganite (birnessite) group, of different chemical composition and crystallinity, and a poorly organized ??-MnO2. All four oxides sorbed significant quantities of silver. The manganous manganites showed the greatest sorption (up to 0.5 moles silver/mole MnOx at pH 7) while the ??-MnO2 showed the least (0.3 moles silver/ mole MnOx at pH 7). Sorption of silver was adequately described by the Langmuir equation over a considerable concentration range. The relationship failed at low pH values and high equilibrium silver concentrations. The sorption capacity showed a direct relationship with pH. However, the rate of increase of sorption capacity decreased at the higher pH values. Silver sorption maxima. were not directly related to surface area but appeared to vary with the amount of occluded sodium and potassium present in the manganese oxide. The important processes involved in the uptake of silver by the four poorly crystallized manganese oxides ara considered to be surface exchange for manganese, potassium and sodium as well as exchange for structural manganese, potassium and sodium. ?? 1973.

  15. Effect of Specimen Thickness on the Creep Response of a Single Crystal Superalloy (Preprint)

    Science.gov (United States)

    2012-01-01

    uncoated specimens of René N5 single crystal super - alloy at a test temperature of 980◦C. In their work coated samples showed higher thickness debit...using a field emission gun (FEI Nova 230) scanning electron microscope (FEGSEM) in order to determine the local texture and microstructural changes, if...shows the presence of damage such as micro-cracks. The internal crack shown in Fig. 7a probably depicts the inter-linkage of big shrinkage pores and

  16. Synthesis of porous CuInS{sub 2} crystals using a stirrer

    Energy Technology Data Exchange (ETDEWEB)

    Akaki, Yoji; Ohno, Yuki; Momiki, Takanori [Miyakonojo National College of Technology, 473-1 Yoshio, Miyakonojo, Miyazaki 885-8567 (Japan)

    2013-08-15

    Porous CuInS{sub 2} crystals were grown from starting materials CuCl{sub 2}.2H{sub 2}O, InCl{sub 3}.4H{sub 2}O and thiorea with ethylene glycol solution, that were placed into a flask, heated, and refluxed for 1 hour. The diffraction peaks only from CuInS{sub 2} phase appear for all the samples. The morphology of CuInS{sub 2} crystal was porous, and the porous crystals exist in two kinds. One kind was flower-like crystals which complexly lack the flakes, another one was sphere-like crystals existed with a number of the poles. The specific surface area of the samples grown by stirring starting materials with In to Cu ratio of 4.3 for 30 minutes was found approximately to be 55 m{sup 2}/g. (copyright 2013 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  17. Anisotropic stress rupture properties of the nickel-base single crystal superalloy SRR99

    International Nuclear Information System (INIS)

    Han, G.M.; Yu, J.J.; Sun, Y.L.; Sun, X.F.; Hu, Z.Q.

    2010-01-01

    The influence of orientation on the stress rupture properties of a single crystal superalloy SRR99 was investigated at temperatures of 760 and 1040 deg. C. It is found that the creep anisotropic behaviour is pronounced at the lower temperature of 760 deg. C and the stress rupture life ranks in the order [0 0 1] > [1 1 1] > [0 1 1]. Despite the anisotropy of stress rupture life is evidently reduced at the higher temperature, the [1 1 1] orientation exhibits the longest life. At 760 deg. C, EBSD (electron back scattered diffraction) was adopted to measure the lattice rotation and the deduced results indicate that the dominant slip systems are {1 1 1} during stress rupture test. At 1040 deg. C, the ranking order of the stress rupture life is [1 1 1] > [0 0 1] > [0 1 1] and the single crystal close to [0 1 1] orientation still shows the poorest life. In the [0 0 1] and [1 1 1] samples, regular γ' raft structure is formed compared with [0 1 1] samples. Further observations made by TEM investigations reveal the underlying deformation mechanisms for crystals with orientations near [0 0 1], [0 1 1] and [1 1 1] under two test conditions.

  18. Analyses of significant features of L-Prolinium Picrate single crystal: An excellent material for non linear optical applications

    Energy Technology Data Exchange (ETDEWEB)

    Thukral, Kanika [Academy of Scientific and Innovative Research, CSIR- National Physical Laboratory, New Delhi, 110012 (India); CSIR-National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi, 110 012 (India); Vijayan, N., E-mail: nvijayan@nplindia.org [CSIR-National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi, 110 012 (India); Vij, Mahak [CSIR-National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi, 110 012 (India); Nagaraja, C.M. [Department of Chemistry, Indian Institute of Technology Ropar, Rupnagar, 140001, Punjab (India); Jayaramakrishnan, V. [Centro De Investigations En Optica, Loma del Bosque 115, Colonia Lomas del Campestre, León, Guanajuato, Código Postal, 37150 (Mexico); Jayalakshmy, M.S. [International and Inter University Centre for Nanoscience and Nanotechnology, Mahatma Gandhi University, Kottayam, Kerala, 686560 (India); Kant, Rajni [Department of Physics and Electronics, University of Jammu, Jammu Tawi, 180006 (India)

    2017-06-15

    Today the fundamental aspect of the researchers is to explore maximum physical properties of the material for device fabrication. In the present article, single crystal X-ray diffraction has been carried out to verify the formation of the synthesized compound. In addition to that, powder X-ray diffraction has been performed to obtain diffraction pattern of L-Prolinium Picrate single crystal. The strain present inside the single crystal was measured using Hall-Williamson equation from PXRD measurements. The dark current and photon current was obtained from photoconductivity technique whose plot depicted that the sample was negative photoconducting material. Optical homogeneity of the single crystal was analyzed using birefringence technique. Its resistance towards Nd: YAG laser was scrutinized for L-Prolinium Picrate single crystal by applying 1 pulse per second. Different thermal parameters like thermal conductivity, thermal diffusivity, thermal effusivity and specific heat were computed using photo-pyroelectric technique. Solid state parameters were calculated from Clausius Mossotti relation by taking structural information of the title compound. Also, optical parameters like refractive index, reflectance etc were calculated through UV–Vis–NIR analysis. - Highlights: • An optically transparent L-Prolinium Picrate single crystal was harvested from slow evaporation solution growth technique. • The compound shows negative photoconducting nature. • Its optical homogeneity was analyzed using birefringence. • Single shot of laser was applied to sample to measure laser damage threshold value. • The thermal parameters were computed from Photopyroelectric technique.

  19. CH3NH3PbCl3 Single Crystals: Inverse Temperature Crystallization and Visible-Blind UV-Photodetector

    KAUST Repository

    Maculan, Giacomo

    2015-09-02

    Single crystals of hybrid perovskites have shown remarkably improved physical properties compared to their polycrystalline film counterparts, underscoring their importance in the further development of advanced semiconductor devices. Here we present a new method of sizeable CH3NH3PbCl3 single crystal growth based on retrograde solubility behavior of hybrid perovskites. We show, for the first time, the energy band structure, charge-carrier recombination and transport properties of single crystal CH3NH3PbCl3. The chloride-based perovskite crystals exhibit trap-state density, charge carriers concentration, mobility and diffusion length comparable with the best quality crystals of methylammonium lead iodide or bromide perovskites reported so far. The high quality of the crystal along with its suitable optical bandgap enabled us to design and build an efficient visible-blind UV-photodetector, demonstrating the potential of this material to be employed in optoelectronic applications.

  20. 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

  1. Report: Independent Environmental Sampling Shows Some Properties Designated by EPA as Available for Use Had Some Contamination

    Science.gov (United States)

    Report #15-P-0221, July 21, 2015. Some OIG sampling results showed contamination was still present at sites designated by the EPA as ready for reuse. This was unexpected and could signal a need to implement changes to ensure human health protection.

  2. Bipolarons in nonmetallic crystals

    International Nuclear Information System (INIS)

    Vinetskii, V.L.; Pashitskii, E.A.; Yanchuk, V.A.

    1987-01-01

    The binding energy of a bipolaron in an ionic crystal increases substantially in the case of strong anisotropy of the effective masses of the free carriers of the easy plane type or easy axis type. In the second case the polaron is cigar-like in shape and the coaxial configuration of bipolarons is energetically favorable. In this case a significant gain in the binding energy and in the width of the region of existence of the bipolaron, with respect to the dielectric constant and the magnitude of the electron-phonon interaction constant, compared with an isotropic crystal, is obtained only for quasi-two-dimensional, or layered, and quasi-one-dimensional, or chainlike, crystals. This work shows that a significant gain in the binding energy can be obtained by taking into account the anisotropy of the dielectric constant of the crystal and localization of the electron wave functions in directions perpendicular to the layers and chains of atoms

  3. Development and melt growth of novel scintillating halide crystals

    Science.gov (United States)

    Yoshikawa, Akira; Yokota, Yuui; Shoji, Yasuhiro; Kral, Robert; Kamada, Kei; Kurosawa, Shunsuke; Ohashi, Yuji; Arakawa, Mototaka; Chani, Valery I.; Kochurikhin, Vladimir V.; Yamaji, Akihiro; Andrey, Medvedev; Nikl, Martin

    2017-12-01

    Melt growth of scintillating halide crystals is reviewed. The vertical Bridgman growth technique is still considered as very popular method that enables production of relatively large and commercially attractive crystals. On the other hand, the micro-pulling-down method is preferable when fabrication of small samples, sufficient for preliminary characterization of their optical and/or scintillation performance, is required. Moreover, bulk crystal growth is also available using the micro-pulling-down furnace. The examples of growths of various halide crystals by industrially friendly melt growth techniques including Czochralski and edge-defined film-fed growth methods are also discussed. Finally, traveling molten zone growth that in some degree corresponds to horizontal zone melting is briefly overviewed.

  4. β-ray irradiation effects in RbBr: Eu crystals

    International Nuclear Information System (INIS)

    Pacheco B, J.M.; Rodriguez M, R.; Perez S, R.

    2006-01-01

    Defects induced by β-ray irradiation in RbBr: Eu 2+ crystals doped with a high concentration of Eu 2+ ions are studied by means of optical absorption (OA), thermoluminescence (TL), and optically stimulated TL (OSTL). The fading, dose, and optical bleaching effects on the TL glow curves of room temperature irradiated samples has been analyzed. OA indicates that irradiation of samples at room temperature induce the formation of F but not F z centers. The TL glow curves show peaks at 267, 303, and 403 K. The 267 K glow peak disappear in less than 1 s under blue light or infrared radiation photo bleaching. A high sensitivity to the ionizing radiation has been observed. These results confirm that this material is an efficient phosphor. (Author)

  5. Effects of post-annealing and cobalt co-doping on superconducting properties of (Ca,Pr)Fe{sub 2}As{sub 2} single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Okada, T., E-mail: 8781303601@mail.ecc.u-tokyo.ac.jp; Ogino, H.; Yakita, H.; Yamamoto, A.; Kishio, K.; Shimoyama, J.

    2014-10-15

    Highlights: • Post-annealing at 400 °C killed superconductivity for Co-free sample. • Pr,Co co-doped samples maintained superconductivity even after annealing. • Two-step superconducting transition was observed via magnetization measurement. • Bulk superconductivity of low-T{sub c} component was confirmed. • Superconducting volume fraction of high-T{sub c} component was always small. - Abstract: In order to clarify the origin of anomalous superconductivity in (Ca,RE)Fe{sub 2}As{sub 2} system, Pr doped and Pr,Co co-doped CaFe{sub 2}As{sub 2} single crystals were grown by the FeAs flux method. These samples showed two-step superconducting transition with T{sub c1} = 25–42 K, and T{sub c2} < 16 K, suggesting that (Ca,RE)Fe{sub 2}As{sub 2} system has two superconducting components. Post-annealing performed for these crystals in evacuated quartz ampoules at various temperatures revealed that post-annealing at ∼400 °C increased the c-axis length for all samples. This indicates that as-grown crystals have a certain level of strain, which is released by post-annealing at ∼400 °C. Superconducting properties also changed dramatically by post-annealing. After annealing at 400 °C, some of the co-doped samples showed large superconducting volume fraction corresponding to the perfect diamagnetism below T{sub c2} and high J{sub c} values of 10{sup 4}–10{sup 5} A cm{sup −2} at 2 K in low field, indicating the bulk superconductivity of (Ca,RE)Fe{sub 2}As{sub 2} phase occurred below T{sub c2}. On the contrary, the superconducting volume fraction above T{sub c2} was always very small, suggesting that 40 K-class superconductivity observed in this system is originating in the local superconductivity in the crystal.

  6. 1. The determination of crystal and magnetic structures

    International Nuclear Information System (INIS)

    Elemans, J.B.A.A.

    1975-01-01

    A theoretical foundation of the technique of thermal neutron scattering by powders is outlined. A description of the experimental set-up is given. A beam of themalized neutrons emerges from the reactor (HFR at Petten) through a slit system. It is diffracted by a manochromator crystal with a finite mosaic structure, a Cu (111) crystal being used. After passing through 10 cm pyrolytic graphite with a ''window'' from 0.23 to 0.29 nm as a lambda/2 filter, resulting in a wave length of 0.257 nm, the neutrons are taken off at a predetermined angle defined by a second slit system, resulting in a beam in which the sample is bathed. The neutrons scattered by the sample are detected by a counter moving in an arc with the position of the sample as center. The standard measurement time for a 10 cm 3 sample was two days. A discussion of the mathematical procedures for deriving the magnetic structure from the observed counts is given

  7. Ferroelectricity and Piezoelectricity in Free-Standing Polycrystalline Films of Plastic Crystals.

    Science.gov (United States)

    Harada, Jun; Yoneyama, Naho; Yokokura, Seiya; Takahashi, Yukihiro; Miura, Atsushi; Kitamura, Noboru; Inabe, Tamotsu

    2018-01-10

    Plastic crystals represent a unique compound class that is often encountered in molecules with globular structures. The highly symmetric cubic crystal structure of plastic crystals endows these materials with multiaxial ferroelectricity that allows a three-dimensional realignment of the polarization axes of the crystals, which cannot be achieved using conventional molecular ferroelectric crystals with low crystal symmetry. In this work, we focused our attention on malleability as another characteristic feature of plastic crystals. We have synthesized the new plastic/ferroelectric ionic crystals tetramethylammonium tetrachloroferrate(III) and tetramethylammonium bromotrichloroferrate(III), and discovered that free-standing translucent films can be easily prepared by pressing powdered samples of these compounds. The thus obtained polycrystalline films exhibit ferroelectric polarization switching and a relatively large piezoelectric response at room temperature. The ready availability of functional films demonstrates the practical utility of such plastic/ferroelectric crystals, and considering the vast variety of possible constituent cations and anions, a wide range of applications should be expected for these unique and attractive functional materials.

  8. Crystallization of modified hydroxyapatite on titanium implants

    International Nuclear Information System (INIS)

    Golovanova, O A; Izmailov, R R; Zaits, A V; Ghyngazov, S A

    2016-01-01

    Carbonated-hydroxyapatite (CHA) and Si-hydroxyapatite (Si-HA) precipitation have been synthesized from the model bioliquid solutions (synovial fluid and SBF). It is found that all the samples synthesized from the model solutions are single-phase and represent hydroxyapatite. The crystallization of the modified hydroxyapatite on alloys of different composition, roughness and subjected to different treatment techniques was investigated. Irradiation of the titanium substrates with the deposited biomimetic coating can facilitate further growth of the crystal and regeneration of the surface. (paper)

  9. Antimicrobial activity and second harmonic studies on organic non-centrosymmetric pure and doped ninhydrin single crystals

    Science.gov (United States)

    Prasanyaa, T.; Jayaramakrishnan, V.; Haris, M.

    2013-03-01

    In this paper, we report the successful growth of pure, Cu2+ ions and Cd2+ ions doped on ninhydrin single crystals by slow solvent evaporation technique. The presence of Cu2+ and Cd2+ ions in the specimen of ninhydrin single crystal has been determined by atomic absorption spectroscopy. The powder X-ray diffraction analysis was done to calculate the lattice parameters of the pure and doped crystals. The percentage of transmittance of the crystal was recorded using the UV-Vis Spectrophotometer. Thermal behaviors of the grown crystals have been examined by the thermal gravimetric/differential thermal analysis. The hardness of the grown crystals was assessed and the results show the minor variation in the hardness value for the pure and doped ninhydrin samples. The value of the work hardening coefficient n was found to be 2.0, 1.0 and 1.06 for pure, copper and cadmium doped ninhydrin crystals respectively. The second harmonic generation efficiency of Cd2+ and Cu2+ doped ninhydrin is 8.3 and 6.3 times greater than well known nonlinear crystal of potassium dihydrogen phosphate respectively. The antibacterial and antifungal activities of the title compound were performed by disk diffusion method against the standard bacteria Escherichia coli, Xanthomonas oryzae and against the fungus Aspergillis niger and Aspergillus flavus.

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

    Science.gov (United States)

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

    2017-07-01

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

  11. The finite-size effect in thin liquid crystal systems

    Science.gov (United States)

    Śliwa, I.

    2018-05-01

    Effects of surface ordering in liquid crystal systems confined between cell plates are of great theoretical and experimental interest. Liquid crystals introduced in thin cells are known to be strongly stabilized and ordered by cell plates. We introduce a new theoretical method for analyzing the effect of surfaces on local molecular ordering in thin liquid crystal systems with planar geometry of the smectic layers. Our results show that, due to the interplay between pair long-range intermolecular forces and nonlocal, relatively short-range, surface interactions, both orientational and translational orders of liquid crystal molecules across confining cells are very complex. In particular, it is demonstrated that the SmA, nematic, and isotropic phases can coexist. The phase transitions from SmA to nematic, as well as from nematic to isotropic phases, occur not simultaneously in the whole volume of the system but begin to appear locally in some regions of the LC sample. Phase transition temperatures are demonstrated to be strongly affected by the thickness of the LC system. The dependence of the corresponding shifts of phase transition temperatures on the layer number is shown to exhibit a power law character. This new type of scaling behavior is concerned with the coexistence of local phases in finite systems. The influence of a specific character of interactions of molecules with surfaces and other molecules on values of the resulting critical exponents is also analyzed.

  12. Crystallization and Melt Removal at Arenal Volcano, Polytopic Vector Analysis

    Science.gov (United States)

    Hidalgo, P. J.; Vogel, T. A.; Bolge, L. L.; Ehrlich, R.; Alvarado, G. E.

    2007-12-01

    enriched end member). Using PVA we refine the interpretations of Bolge and coworkers and show that melt from the crystalline rich ET3 tephra was removed and ponded in the magma chamber above the crystalline mush (top part of ET4 unit). Thus when the eruption occurred the most evolved tephra (ET4) were deposited first followed by the least evolved tephra (ET3), which resulted in sampling of a chemically zoned magma chamber. Using PVA on stratigraphically controlled whole-rock analyses of tephra samples, we can unambiguously identify processes and end members that are involved in crystal accumulation and liquid separation processes. Thus PVA is a rigorous analytical tool that uses only whole-rock chemical data to produce robust results that can be used with other analytical techniques to test petrological models.

  13. Demonstrations with a Liquid Crystal Shutter

    Science.gov (United States)

    Kraftmakher, Yaakov

    2012-01-01

    The experiments presented show the response of a liquid crystal shutter to applied electric voltages and the delay of the operations. Both properties are important for liquid crystal displays of computers and television sets. Two characteristics of the shutter are determined: (i) the optical transmittance versus applied voltage of various…

  14. X-ray fluorescence holography studies for a Cu3Au crystal

    Science.gov (United States)

    Dąbrowski, K. M.; Dul, D. T.; Jaworska-Gołąb, T.; Rysz, J.; Korecki, P.

    2015-12-01

    In this work we show that performing a numerical correction for beam attenuation and indirect excitation allows one to fully restore element sensitivity in the three-dimensional reconstruction of the atomic structure. This is exemplified by a comparison of atomic images reconstructed from holograms measured for ordered and disordered phases of a Cu3Au crystal that clearly show sensitivity to changes in occupancy of the atomic sites. Moreover, the numerical correction, which is based on quantitative methods of X-ray fluorescence spectroscopy, was extended to take into account the influence of a disturbed overlayer in the sample.

  15. Nd-doped Lu3Al5O12 single-crystal scintillator for X-ray imaging

    International Nuclear Information System (INIS)

    Sugiyama, Makoto; Fujimoto, Yutaka; Yanagida, Takayuki; Totsuka, Daisuke; Chani, Valery; Yokota, Yuui; Yoshikawa, Akira

    2013-01-01

    The optical and scintillation properties of Nd-doped Lu 3 Al 5 O 12 (Nd:LuAG) crystals grown by the Czochralski (Cz) method were examined under X-ray excitation. Their applicability for X-ray imaging was also inspected. The radioluminescence spectrum induced by X-rays showed a broad host emission and sharp Nd 3+ 4f–4f emission peaks in the UV to visible wavelengths. The light output current of the Nd:LuAG was 85% of that of a standard CdWO 4 X-ray scintillator. The afterglow value measured 20 ms after X-ray irradiation was 1.5%. An X-ray radiographic image was successfully obtained using the Nd:LuAG scintillator coupled with the charge coupled device (CCD) photodetector. -- Highlights: ► The Nd:LuAG single crystal was produced to perform X-ray imaging test. ► The sample exhibited the 85% light output current of the standard CdWO 4 . ► The afterglow intensity of the sample was very high compared with the CdWO 4 . ► The X-ray radiographic image was obtained from the Nd:LuAG single crystal

  16. Crystallization of carbohydrate oxidase from Microdochium nivale

    International Nuclear Information System (INIS)

    Dušková, Jarmila; Dohnálek, Jan; Skálová, Tereza; Østergaard, Lars Henrik; Fuglsang, Claus Crone; Kolenko, Petr; Štěpánková, Andrea; Hašek, Jindřich

    2009-01-01

    Industrially used carbohydrate oxidase was successfully crystallized in several forms, diffraction data suitable for structural analysis were collected. Microdochium nivale carbohydrate oxidase was produced by heterologous recombinant expression in Aspergillus oryzae, purified and crystallized. The enzyme crystallizes with varying crystal morphologies depending on the crystallization conditions. Several different crystal forms were obtained using the hanging-drop vapour-diffusion method, two of which were used for diffraction measurements. Hexagon-shaped crystals (form I) diffracted to 2.66 Å resolution, with unit-cell parameters a = b = 55.7, c = 610.4 Å and apparent space group P6 2 22. Analysis of the data quality showed almost perfect twinning of the crystals. Attempts to solve the structure by molecular replacement did not give satisfactory results. Recently, clusters of rod-shaped crystals (form II) were grown in a solution containing PEG MME 550. These crystals belonged to the monoclinic system C2, with unit-cell parameters a = 132.9, b = 56.6, c = 86.5 Å, β = 95.7°. Data sets were collected to a resolution of 2.4 Å. The structure was solved by the molecular-replacement method. Model refinement is currently in progress

  17. Unidirectional Wave Propagation in Low-Symmetric Colloidal Photonic-Crystal Heterostructures

    Directory of Open Access Journals (Sweden)

    Vassilios Yannopapas

    2015-03-01

    Full Text Available We show theoretically that photonic crystals consisting of colloidal spheres exhibit unidirectional wave propagation and one-way frequency band gaps without breaking time-reversal symmetry via, e.g., the application of an external magnetic field or the use of nonlinear materials. Namely, photonic crystals with low symmetry such as the monoclinic crystal type considered here as well as with unit cells formed by the heterostructure of different photonic crystals show significant unidirectional electromagnetic response. In particular, we show that the use of scatterers with low refractive-index contrast favors the formation of unidirectional frequency gaps which is the optimal route for achieving unidirectional wave propagation.

  18. Unidirectional Wave Propagation in Low-Symmetric Colloidal Photonic-Crystal Heterostructures.

    Science.gov (United States)

    Yannopapas, Vassilios

    2015-03-19

    We show theoretically that photonic crystals consisting of colloidal spheres exhibit unidirectional wave propagation and one-way frequency band gaps without breaking time-reversal symmetry via, e.g., the application of an external magnetic field or the use of nonlinear materials. Namely, photonic crystals with low symmetry such as the monoclinic crystal type considered here as well as with unit cells formed by the heterostructure of different photonic crystals show significant unidirectional electromagnetic response. In particular, we show that the use of scatterers with low refractive-index contrast favors the formation of unidirectional frequency gaps which is the optimal route for achieving unidirectional wave propagation.

  19. Trapezoidal diffraction grating beam splitters in single crystal diamond

    Science.gov (United States)

    Kiss, Marcell; Graziosi, Teodoro; Quack, Niels

    2018-02-01

    Single Crystal Diamond has been recognized as a prime material for optical components in high power applications due to low absorption and high thermal conductivity. However, diamond microstructuring remains challenging. Here, we report on the fabrication and characterization of optical diffraction gratings exhibiting a symmetric trapezoidal profile etched into a single crystal diamond substrate. The optimized grating geometry diffracts the transmitted optical power into precisely defined proportions, performing as an effective beam splitter. We fabricate our gratings in commercially available single crystal CVD diamond plates (2.6mm x 2.6mm x 0.3mm). Using a sputter deposited hard mask and patterning by contact lithography, the diamond is etched in an inductively coupled oxygen plasma with zero platen power. The etch process effectively reveals the characteristic {111} diamond crystal planes, creating a precisely defined angled (54.7°) profile. SEM and AFM measurements of the fabricated gratings evidence the trapezoidal shape with a pitch of 3.82μm, depth of 170 nm and duty cycle of 35.5%. Optical characterization is performed in transmission using a 650nm laser source perpendicular to the sample. The recorded transmitted optical power as function of detector rotation angle shows a distribution of 21.1% in the 0th order and 23.6% in each +/-1st order (16.1% reflected, 16.6% in higher orders). To our knowledge, this is the first demonstration of diffraction gratings with trapezoidal profile in single crystal diamond. The fabrication process will enable beam splitter gratings of custom defined optical power distribution profiles, while antireflection coatings can increase the efficiency.

  20. N and Si Implantation Effect on Structural and Electrical Properties of Bridgman grown GaSe Single Crystal

    International Nuclear Information System (INIS)

    Karabulut, O.

    2004-01-01

    N and Si implantation to GaSe single crystals were carried out parallel to c-axis with ion beam of about 10 1 6 ions/cm 2 dose having energy values 30, 60 and 100 keV. Ion implantation modifications on Bridgman grown GaSe single crystals have been investigated by means of XRD, electrical conductivity, absorption and photoconductivity measurements. XRD measurements revealed that annealing results in a complete recovery of the crystalline nature that was moderately reduced upon implantation. It was observed that both N- and Siimplantation followed by annealing process decreased the resistivity values from 10 7 to 10 3 .-cm. The analysis of temperature dependent conductivity showed that at high temperature region above 200 K, the transport mechanism is dominated by thermal excitation in the doped and undoped GaSe samples. At lower temperatures, the conduction of carriers is dominated by variable range hopping mechanism in the implanted samples. Absorption and spectral photoconductivity measurements showed that the band edge is shifted in the implanted sample. All these modifications were attributed to the structural modifications and continuous shallow trap levels introduced upon implantation and annealing

  1. Direct investigations on strain-induced cold crystallization behavior and structure evolutions in amorphous poly(lactic acid) with SAXS and WAXS measurements

    DEFF Research Database (Denmark)

    Zhou, Chengbo; Li, Hongfei; Zhang, Wenyang

    2016-01-01

    scanning calorimetry (DSC) measurements. The data obtained from the stretched samples within 70-90 degrees C showed that all of the formed crystals are disordered alpha' form with more compact chain packing than that of the cold crystallization. Upon stretching at 70 degrees C, the mesocrystal appears......Strain-induced cold crystallization behavior and structure evolution of amorphous poly(lactic acid) (PLA) stretched within 70-90 degrees C were investigated via in situ synchrotron small-angle X-ray scattering (SAXS) and wide-angle X-ray scattering (WAXS) measurements as well as differential...... in strain-induced crystallization behavior of amorphous PLA within 70-90 degrees C can be attributed to the competition between chain orientation caused by stretching and chain relaxation. It was proposed that the strain-induced mesocrystal/crystal and the lamellae are formed from the mesophase originally...

  2. Hydrothermal Growth of Polyscale Crystals

    Science.gov (United States)

    Byrappa, Kullaiah

    In this chapter, the importance of the hydrothermal technique for growth of polyscale crystals is discussed with reference to its efficiency in synthesizing high-quality crystals of various sizes for modern technological applications. The historical development of the hydrothermal technique is briefly discussed, to show its evolution over time. Also some of the important types of apparatus used in routine hydrothermal research, including the continuous production of nanosize crystals, are discussed. The latest trends in the hydrothermal growth of crystals, such as thermodynamic modeling and understanding of the solution chemistry, are elucidated with appropriate examples. The growth of some selected bulk, fine, and nanosized crystals of current technological significance, such as quartz, aluminum and gallium berlinites, calcite, gemstones, rare-earth vanadates, electroceramic titanates, and carbon polymorphs, is discussed in detail. Future trends in the hydrothermal technique, required to meet the challenges of fast-growing demand for materials in various technological fields, are described. At the end of this chapter, an Appendix 18.A containing a more or less complete list of the characteristic families of crystals synthesized by the hydrothermal technique is given with the solvent and pressure-temperature (PT) conditions used in their synthesis.

  3. Role of Absorbing Nanocrystal Cores in Soft Photonic Crystals: A Spectroscopy and SANS Study.

    Science.gov (United States)

    Rauh, Astrid; Carl, Nico; Schweins, Ralf; Karg, Matthias

    2018-01-23

    Periodic superstructures of plasmonic nanoparticles have attracted significant interest because they can support coupled plasmonic modes, making them interesting for plasmonic lasing, metamaterials, and as light-management structures in thin-film optoelectronic devices. We have recently shown that noble metal hydrogel core-shell colloids allow for the fabrication of highly ordered 2-dimensional plasmonic lattices that show surface lattice resonances as the result of plasmonic/diffractive coupling (Volk, K.; Fitzgerald, J. P. S.; Ruckdeschel, P.; Retsch, M.; König, T. A. F.; Karg, M. Reversible Tuning of Visible Wavelength Surface Lattice Resonances in Self-Assembled Hybrid Monolayers. Adv. Optical Mater. 2017, 5, 1600971, DOI: 10.1002/adom.201600971). In the present work, we study the photonic properties and structure of 3-dimensional crystalline superstructures of gold hydrogel core-shell colloids and their pitted counterparts without gold cores. We use far-field extinction spectroscopy to investigate the optical response of these superstructures. Narrow Bragg peaks are measured, independently of the presence or absence of the gold cores. All crystals show a significant reduction in low-wavelength scattering. This leads to a significant enhancement of the plasmonic properties of the samples prepared from gold-nanoparticle-containing core-shell colloids. Plasmonic/diffractive coupling is not evident, which we mostly attribute to the relatively small size of the gold cores limiting the effective coupling strength. Small-angle neutron scattering is applied to study the crystal structure. Bragg peaks of several orders clearly assignable to an fcc arrangement of the particles are observed for all crystalline samples in a broad range of volume fractions. Our results indicate that the nanocrystal cores do not influence the overall crystallization behavior or the crystal structure. These are important prerequisites for future studies on photonic materials built from core

  4. The effect of deformation twinning on irradiation embrittlement in iron single crystals

    International Nuclear Information System (INIS)

    Kayano, Hideo; Tokutomi, Shoichiro; Yajima, Seishi; Takaku, Hiroshi.

    1978-01-01

    Single crystals of iron with the [100] crystal orientation were irradiated in JMTR with fast neutrons to a fluence of 8 x 10 18 n/cm 2 (E > 1 MeV). All samples were deformed in tension at temperatures from liquid nitrogen temperature to 200 0 C at different strain rates using an Instron-type tensile testing machine. Scanning electron microscopy of the fractured surfaces revealed that deformation twinning is difficult to occur in irradiated samples, and also that twins formed in both irradiated and unirradiated samples inhibit fracture nucleation and growth. From the results of tensile deformation of the irradiated samples deformed in tension a different strain rates at 159 0 K, it is conceived that twinning suppression is greater in the irradiated than in the unirradiated samples, and that the nucleation and growth of twins are not necessarily related to those of cracks. It is suggested that the irradiation-induced defects impede plastic deformation of the crystals and deformation twinning is suppressed by irradiation, thus causing the irradiation embrittlement. (auth.)

  5. Creation of tunable absolute bandgaps in a two-dimensional anisotropic photonic crystal modulated by a nematic liquid crystal

    International Nuclear Information System (INIS)

    Liu Chenyang

    2008-01-01

    Photonic crystals (PCs) have many potential applications because of their ability to control light-wave propagation. We have investigated the tunable absolute bandgap in a two-dimensional anisotropic photonic crystal structures modulated by a nematic liquid crystal. The PC structure composed of an anisotropic-dielectric cylinder in the liquid crystal medium is studied by solving Maxwell's equations using the plane wave expansion method. The photonic band structures are found to exhibit absolute bandgaps for the square and triangular lattices. Numerical simulations show that the absolute bandgaps can be continuously tuned in the square and triangular lattices consisting of anisotropic-dielectric cylinders by infiltrating nematic liquid crystals. Such a mechanism of bandgap adjustment should open up a new application for designing components in photonic integrated circuits

  6. Crystallization of aqueous ammonium sulfate particles internally mixed with soot and kaolinite: crystallization relative humidities and nucleation rates.

    Science.gov (United States)

    Pant, Atul; Parsons, Matthew T; Bertram, Allan K

    2006-07-20

    Using optical microscopy, we investigated the crystallization of aqueous ammonium sulfate droplets containing soot and kaolinite, as well as the crystallization of aqueous ammonium sulfate droplets free of solid material. Our results show that soot did not influence the crystallization RH of aqueous ammonium sulfate particles under our experimental conditions. In contrast, kaolinite increased the crystallization RH of the aqueous ammonium sulfate droplets by approximately 10%. In addition, our results show that the crystallization RH of aqueous ammonium sulfate droplets free of solid material does not depend strongly on particle size. This is consistent with conclusions made previously in the literature, based on comparisons of results from different laboratories. From the crystallization results we determined the homogeneous nucleation rates of crystalline ammonium sulfate in aqueous ammonium sulfate droplets and the heterogeneous nucleation rates of crystalline ammonium sulfate in aqueous ammonium sulfate particles containing kaolinite. Using classical nucleation theory and our experimental data, we determined that the interfacial tension between an ammonium sulfate critical nucleus and an aqueous ammonium sulfate solution is 0.064 +/- 0.003 J m(-2) (in agreement with our previous measurements), and the contact angle between an ammonium sulfate critical nucleus and a kaolinite surface is 59 +/- 2 degrees. On the basis of our results, we argue that soot will not influence the crystallization RH of aqueous ammonium sulfate droplets in the atmosphere, but kaolinite can significantly modify the crystallization RH of atmospheric ammonium sulfate droplets. As an example, the CRH50 (the relative humidity at which 50% of the droplets crystallize) ranges from about 41 to 51% RH when the diameter of the kaolinite inclusion ranges from 0.1 to 5 microm. For comparison, the CRH50 of aqueous ammonium sulfate droplets (0.5 microm diameter) free of solid material is

  7. Coupled Photonic Crystal Cavity Array Laser

    DEFF Research Database (Denmark)

    Schubert, Martin

    in the quadratic lattice. Processing techniques are developed and optimized in order fabricate photonic crystals membranes in gallium arsenide with quantum dots as gain medium and in indium gallium arsenide phosphide with quantum wells as gain medium. Several key issues in process to ensure good quality....... The results are in good agreement with standard coupled mode theory. Also a novel type of photonic crystal structure is proposed called lambda shifted cavity which is a twodimensional photonic crystal laser analog of a VCSEL laser. Detailed measurements of the coupled modes in the photonic crystals...... with quantum dots are carried out. In agreement with a simple gain model the structures do not show stimulated emission. The spectral splitting due to the coupling between single cavities as well as arrays of cavities is studied theoretically and experimentally. Lasing is observed for photonic crystal cavity...

  8. Effect of nanoclay on the nonisothermal crystallization of poly(propylene) and its blend with poly[(butylene succinate)-co-adipate

    CSIR Research Space (South Africa)

    Bandyopadhyay, J

    2012-05-01

    Full Text Available and nanoclay modified PP/PBSA blend composite samples was evaluated by using Kissinger and Augis-Bennett methods. The results showed that the absolute value of the activation energy for the PP matrix crystallization was increased in the case of PP/PBSA blend...

  9. Crystallization of Trehalose in Frozen Solutions and its Phase Behavior during Drying

    Energy Technology Data Exchange (ETDEWEB)

    Sundaramurthi, Prakash; Patapoff, Thomas W.; Suryanarayanan, Raj (Genentech); (UMM)

    2015-02-19

    To study the crystallization of trehalose in frozen solutions and to understand the phase transitions during the entire freeze-drying cycle. Aqueous trehalose solution was cooled to -40 C in a custom-designed sample holder. The frozen solution was warmed to -18 C and annealed, and then dried in the sample chamber of the diffractometer. XRD patterns were continuously collected during cooling, annealing and drying. After cooling, hexagonal ice was the only crystalline phase observed. However, upon annealing, crystallization of trehalose dihydrate was evident. Seeding the frozen solution accelerated the solute crystallization. Thus, phase separation of the lyoprotectant was observed in frozen solutions. During drying, dehydration of trehalose dihydrate yielded a substantially amorphous anhydrous trehalose. Crystallization of trehalose, as trehalose dihydrate, was observed in frozen solutions. The dehydration of the crystalline trehalose dihydrate to substantially amorphous anhydrate occurred during drying. Therefore, analyzing the final lyophile will not reveal crystallization of the lyoprotectant during freeze-drying. The lyoprotectant crystallization can only become evident by continuous monitoring of the system during the entire freeze-drying cycle. In light of the phase separation of trehalose in frozen solutions, its ability to serve as a lyoprotectant warrants further investigation.

  10. Crystal structure solution of hydrides containing natEu from neutron powder diffraction data

    International Nuclear Information System (INIS)

    Kohlmann, H.

    1999-01-01

    Complete text of publication follows. The location of hydrogen in crystal structures of metal hydrides usually requires neutron diffraction data. Some elements, however, show excessively high absorption cross sections, σ a , for neutrons, thus making this technique seemingly impractical. Therefore no complete, refined crystal structure data of europium hydrides (σ a ( nat Eu) = .4530 barns at λ = 179.8 pm [1]) have been reported so far. It is shown that the absorption can be reduced to a value reasonable for neutron diffraction experiments by taking advantage of the wavelength dependence of σ a combined with the use of annular samples at advanced diffractometers. Neutron powder diffraction data on several nat Eu containing deuterides suitable for the ab initio crystal structure solution and refinement have been taken at D20 and D4 (ILL, Grenoble). The crystal chemistry of these europium hydrides, among them the two new compounds EuMg 2 H 6 and EuMgH 4 [2], is discussed. (author) [1] V.F. Sears, Neutron News 1992, 3, 26-37.; [2] H. Kohlmann, F. Gingl, T. Hansen, K. Yvon, Angew. Chem. Int. Ed. Eng. 1999, 38, accepted

  11. Crystal-field magnetic anisotropy of dilute dysprosium or erbium in yttrium single crystals

    DEFF Research Database (Denmark)

    Høg, J.; Touborg, P.

    1974-01-01

    Magnetization measurements have been performed between 1.3 and 300 K in fields up to 50 × 105 A/m in the a, b, and c directions of hcp crystals of pure Y and Y doped with 0.14-at.% Dy or 0.14-at.% Er, using the Faraday method and a vibrating-sample method. The characteristic behavior of both...

  12. Development of an X-ray fluorescence holographic measurement system for protein crystals

    Energy Technology Data Exchange (ETDEWEB)

    Sato-Tomita, Ayana, E-mail: ayana.sato@jichi.ac.jp, E-mail: shibayam@jichi.ac.jp, E-mail: hayashi.koichi@nitech.ac.jp; Shibayama, Naoya, E-mail: ayana.sato@jichi.ac.jp, E-mail: shibayam@jichi.ac.jp, E-mail: hayashi.koichi@nitech.ac.jp; Okabe, Takahiro [Division of Biophysics, Department of Physiology, Jichi Medical University, Yakushiji, Shimotsuke 329-0498 (Japan); Happo, Naohisa [Department of Computer and Network Engineering, Graduate School of Information Sciences, Hiroshima City University, Asa-Minami-Ku, Hiroshima 731-3194 (Japan); Kimura, Koji [Department of Physical Science and Engineering, Nagoya Institute of Technology, Gokiso, Showa, Nagoya 466-8555 (Japan); Matsushita, Tomohiro [Japan Synchrotron Radiation Research Institute (JASRI), SPring-8, Sayo, Hyogo 679-5198 (Japan); Park, Sam-Yong [Drug Design Laboratory, Department of Medical Life Science, Yokohama City University, Suehiro, Tsurumi, Yokohama 230-0045 (Japan); Sasaki, Yuji C. [Department of Advanced Material Science, Graduate School of Frontier Science, The University of Tokyo, Kashiwanoha, Kashiwa 277-8561 (Japan); Hayashi, Kouichi, E-mail: ayana.sato@jichi.ac.jp, E-mail: shibayam@jichi.ac.jp, E-mail: hayashi.koichi@nitech.ac.jp [Department of Physical Science and Engineering, Nagoya Institute of Technology, Gokiso, Showa, Nagoya 466-8555 (Japan); Frontier Research Institute for Materials Science, Nagoya Institute of Technology, Gokiso, Showa, Nagoya 466-8555 (Japan)

    2016-06-15

    Experimental procedure and setup for obtaining X-ray fluorescence hologram of crystalline metalloprotein samples are described. Human hemoglobin, an α{sub 2}β{sub 2} tetrameric metalloprotein containing the Fe(II) heme active-site in each chain, was chosen for this study because of its wealth of crystallographic data. A cold gas flow system was introduced to reduce X-ray radiation damage of protein crystals that are usually fragile and susceptible to damage. A χ-stage was installed to rotate the sample while avoiding intersection between the X-ray beam and the sample loop or holder, which is needed for supporting fragile protein crystals. Huge hemoglobin crystals (with a maximum size of 8 × 6 × 3 mm{sup 3}) were prepared and used to keep the footprint of the incident X-ray beam smaller than the sample size during the entire course of the measurement with the incident angle of 0°-70°. Under these experimental and data acquisition conditions, we achieved the first observation of the X-ray fluorescence hologram pattern from the protein crystals with minimal radiation damage, opening up a new and potential method for investigating the stereochemistry of the metal active-sites in biomacromolecules.

  13. Crystal structure analysis, overexpression and refolding behaviour of a DING protein with single mutation

    International Nuclear Information System (INIS)

    Gai, Zuoqi; Nakamura, Akiyoshi; Tanaka, Yoshikazu; Hirano, Nagisa; Tanaka, Isao; Yao, Min

    2013-01-01

    Crystals of a member of the DING protein family (HPBP) were obtained accidentally, and the structure was determined at 1.35 Å resolution. For further analysis, a system for preparation of HPBP was constructed and the structure of a prepared sample was confirmed by X-ray crystal structure analysis at 1.03 Å resolution. After crystallization of a certain protein–RNA complex, well diffracting crystals were obtained. However, the asymmetric unit of the crystal was too small to locate any components. Mass spectrometry and X-ray crystal structure analysis showed that it was a member of the DING protein family (HPBP). Surprisingly, the structure of HPBP reported previously was also determined accidentally as a contaminant, suggesting that HPBP has a strong tendency to crystallize. Furthermore, DING proteins were reported to relate in disease. These observations suggest that DING has potential for application in a wide range of research fields. To enable further analyses, a system for preparation of HPBP was constructed. As HPBP was expressed in insoluble form in Escherichia coli, it was unfolded chemically and refolded. Finally, a very high yield preparation method was constructed, in which 43 mg of HPBP was obtained from 1 L of culture. Furthermore, to evaluate the validity of refolding, its crystal structure was determined at 1.03 Å resolution. The determined structure was identical to the native structure, in which two disulfide bonds were recovered correctly and a phosphate ion was captured. Based on these results, it was concluded that the refolded HPBP recovers its structure correctly

  14. Crystal structure analysis, overexpression and refolding behaviour of a DING protein with single mutation

    Energy Technology Data Exchange (ETDEWEB)

    Gai, Zuoqi; Nakamura, Akiyoshi [Hokkaido University, Sapporo 060-0810 (Japan); Tanaka, Yoshikazu, E-mail: tanaka@sci.hokudai.ac.jp [Hokkaido University, Sapporo 060-0810 (Japan); Hokkaido University, Sapporo 060-0810 (Japan); Hirano, Nagisa [Hokkaido University, Sapporo 060-0810 (Japan); Tanaka, Isao; Yao, Min [Hokkaido University, Sapporo 060-0810 (Japan); Hokkaido University, Sapporo 060-0810 (Japan)

    2013-11-01

    Crystals of a member of the DING protein family (HPBP) were obtained accidentally, and the structure was determined at 1.35 Å resolution. For further analysis, a system for preparation of HPBP was constructed and the structure of a prepared sample was confirmed by X-ray crystal structure analysis at 1.03 Å resolution. After crystallization of a certain protein–RNA complex, well diffracting crystals were obtained. However, the asymmetric unit of the crystal was too small to locate any components. Mass spectrometry and X-ray crystal structure analysis showed that it was a member of the DING protein family (HPBP). Surprisingly, the structure of HPBP reported previously was also determined accidentally as a contaminant, suggesting that HPBP has a strong tendency to crystallize. Furthermore, DING proteins were reported to relate in disease. These observations suggest that DING has potential for application in a wide range of research fields. To enable further analyses, a system for preparation of HPBP was constructed. As HPBP was expressed in insoluble form in Escherichia coli, it was unfolded chemically and refolded. Finally, a very high yield preparation method was constructed, in which 43 mg of HPBP was obtained from 1 L of culture. Furthermore, to evaluate the validity of refolding, its crystal structure was determined at 1.03 Å resolution. The determined structure was identical to the native structure, in which two disulfide bonds were recovered correctly and a phosphate ion was captured. Based on these results, it was concluded that the refolded HPBP recovers its structure correctly.

  15. Automated sample mounting and technical advance alignment system for biological crystallography at a synchrotron source

    International Nuclear Information System (INIS)

    Snell, Gyorgy; Cork, Carl; Nordmeyer, Robert; Cornell, Earl; Meigs, George; Yegian, Derek; Jaklevic, Joseph; Jin, Jian; Stevens, Raymond C.; Earnest, Thomas

    2004-01-01

    High-throughput data collection for macromolecular crystallography requires an automated sample mounting system for cryo-protected crystals that functions reliably when integrated into protein-crystallography beamlines at synchrotrons. Rapid mounting and dismounting of the samples increases the efficiency of the crystal screening and data collection processes, where many crystals can be tested for the quality of diffraction. The sample-mounting subsystem has random access to 112 samples, stored under liquid nitrogen. Results of extensive tests regarding the performance and reliability of the system are presented. To further increase throughput, we have also developed a sample transport/storage system based on 'puck-shaped' cassettes, which can hold sixteen samples each. Seven cassettes fit into a standard dry shipping Dewar. The capabilities of a robotic crystal mounting and alignment system with instrumentation control software and a relational database allows for automated screening and data collection to be developed

  16. Optical studies of metallo-dielectric photonic crystals

    Science.gov (United States)

    Kamaev, Vladimir

    2007-12-01

    Metallo-dielectric photonic crystals (MDPCs) are characterized by a large difference between the dielectric constants of the constituents. Owing to their high DC conductivity a broad omnidirectional band gap is formed at low frequencies. At the same time there exist numerous propagating electromagnetic modes at frequencies above a cutoff. This gives a possibility of creating a "transparent" metal: a crystal transparent in the visible spectral range and simultaneously having high DC conductivity. Since the cutoff wavelength linearly scales with the crystal periodicity, in order to make an MDPC with propagating modes in the visible range the crystal periodicity has to be around a quarter micrometer. Fabrication of such a crystal is a challenging task. One of the feasible choices is natural or artificial opals, structures made of silica balls arranged into a close packed fcc lattice. The ball diameters could vary from 200 nm to several microns, allowing the desired optical features to be in the visible spectral range. In the present work we studied metal-infiltrated opals numerically, analytically, and experimentally (Chapters 1 and 4). Both theory and experiment revealed high reflectance of the samples at large wavelengths associated with the low frequency metallic band gap formation, and low reflectance at short wavelengths that has characteristic wiggles. Contrarily, the absorbance is low in the IR region and goes up towards the UV end, which is due to low group velocity of light and high metal absorption in the region. Numerical analysis of thin metal-infiltrated opals (˜3-5 layers) did show a transmission peak around the first reflectance minimum and cutoff frequency. In Chapter 5 we present transmission experiments on thin metal films perforated with periodic arrays of holes or deposited on an opal monolayer. Both types of 2D MDPCs exhibited anomalous transmission peaks associated with surface plasma excitations. It was shown that the phenomenon could be

  17. The thickness of native oxides on aluminum alloys and single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Evertsson, J., E-mail: jonas.evertsson@sljus.lu.se [Division of Synchrotron Radiation Research, Lund University, Box 118, 221 00 Lund (Sweden); Bertram, F. [Division of Synchrotron Radiation Research, Lund University, Box 118, 221 00 Lund (Sweden); Zhang, F. [KTH Royal Institute of Technology, Department of Chemistry, Division of Surface and Corrosion Science, Drottning Kristinas Vg 51, 100 44 Stockholm (Sweden); Rullik, L.; Merte, L.R.; Shipilin, M. [Division of Synchrotron Radiation Research, Lund University, Box 118, 221 00 Lund (Sweden); Soldemo, M.; Ahmadi, S. [KTH Royal Institute of Technology, ICT, Material Physics, 16440 Kista (Sweden); Vinogradov, N.; Carlà, F. [ESRF, B.P. 220, 38043 Grenoble (France); Weissenrieder, J.; Göthelid, M. [KTH Royal Institute of Technology, ICT, Material Physics, 16440 Kista (Sweden); Pan, J. [KTH Royal Institute of Technology, Department of Chemistry, Division of Surface and Corrosion Science, Drottning Kristinas Vg 51, 100 44 Stockholm (Sweden); Mikkelsen, A. [Division of Synchrotron Radiation Research, Lund University, Box 118, 221 00 Lund (Sweden); Nilsson, J.-O. [Sapa Technology, Kanalgatan 1, 612 31 Finspång (Sweden); Lundgren, E. [Division of Synchrotron Radiation Research, Lund University, Box 118, 221 00 Lund (Sweden)

    2015-09-15

    Highlights: • We have determined the native oxide film thickness on several Al samples. • The results obtained from XRR and XPS show excellent agreement. • The results obtained from EIS show consistently thinner oxide films. • The oxides on the alloys are thicker than the oxides on the single crystals. - Abstract: We present results from measurements of the native oxide film thickness on four different industrial aluminum alloys and three different aluminum single crystals. The thicknesses were determined using X-ray reflectivity, X-ray photoelectron spectroscopy, and electrochemical impedance spectroscopy. In addition, atomic force microscopy was used for micro-structural studies of the oxide surfaces. The reflectivity measurements were performed in ultra-high vacuum, vacuum, ambient, nitrogen and liquid water conditions. The results obtained using X-ray reflectivity and X-ray photoelectron spectroscopy demonstrate good agreement. However, the oxide thicknesses determined from the electrochemical impedance spectroscopy show a larger discrepancy from the above two methods. In the present contribution the reasons for this discrepancy are discussed. We also address the effect of the substrate type and the presence of water on the resultant oxide thickness.

  18. Twinning of Polymer Crystals Suppressed by Entropy

    Directory of Open Access Journals (Sweden)

    Nikos Ch. Karayiannis

    2014-09-01

    Full Text Available We propose an entropic argument as partial explanation of the observed scarcity of twinned structures in crystalline samples of synthetic organic polymeric materials. Polymeric molecules possess a much larger number of conformational degrees of freedom than low molecular weight substances. The preferred conformations of polymer chains in the bulk of a single crystal are often incompatible with the conformations imposed by the symmetry of a growth twin, both at the composition surfaces and in the twin axis. We calculate the differences in conformational entropy between chains in single crystals and chains in twinned crystals, and find that the reduction in chain conformational entropy in the twin is sufficient to make the single crystal the stable thermodynamic phase. The formation of cyclic twins in molecular dynamics simulations of chains of hard spheres must thus be attributed to kinetic factors. In more realistic polymers this entropic contribution to the free energy can be canceled or dominated by nonbonded and torsional energetics.

  19. Crystallization of hard spheres revisited. II. Thermodynamic modeling, nucleation work, and the surface of tension.

    Science.gov (United States)

    Richard, David; Speck, Thomas

    2018-06-14

    Combining three numerical methods (forward flux sampling, seeding of droplets, and finite-size droplets), we probe the crystallization of hard spheres over the full range from close to coexistence to the spinodal regime. We show that all three methods allow us to sample different regimes and agree perfectly in the ranges where they overlap. By combining the nucleation work calculated from forward flux sampling of small droplets and the nucleation theorem, we show how to compute the nucleation work spanning three orders of magnitude. Using a variation of the nucleation theorem, we show how to extract the pressure difference between the solid droplet and ambient liquid. Moreover, combining the nucleation work with the pressure difference allows us to calculate the interfacial tension of small droplets. Our results demonstrate that employing bulk quantities yields inaccurate results for the nucleation rate.

  20. NONLINEAR OPTICAL MOLECULAR CRYSTAL BASED ON 2,6-DIAMINOPYRIDINE: SYNTHESIS AND CHARACTERIZATION

    Directory of Open Access Journals (Sweden)

    I. M. Pavlovetc

    2014-05-01

    Full Text Available The paper deals with investigation of a new nonlinear optical material based on nonlinear optical chromophore (4-Nitrophenol and aminopyridine (2,6-Diaminopyridine. Calculation results are presented for molecular packing in the crystalline compound, based on the given components. According to these results the finite material must have a noncentrosymmetric lattice, which determines the presence of the second order nonlinear optical response. Investigations carried out in this work confirm these calculations. Results of experiments are given describing the co-crystallization of these components and the following re-crystallization of the obtained material. In order to get a monocrystal form, the optimal conditions for the synthesis of molecular crystals based on these components are determined. Sufficiently large homogeneous crystals are obtained, that gave the possibility to record their spectra in the visible and near infrared parts of the spectrum, to determine their nonlinear optical properties and the level of homogeneity. Their optical (optical transmission and optical laser damage threshold and nonlinear optical properties are presented. For observation and measurement of the nonlinear optical properties an installation was built which implements the comparative method for measurements of nonlinear optical properties. A potassium titanyl oxide phosphate crystal was used as a sample for comparison. Results are given for the conversion efficiency of the primary laser radiation in the second optical harmonic relative to the signal obtained on the potassium titanyl oxide phosphate crystal. Obtained results show that the molecular co-crystal based on 2,6-Diaminopyridine is a promising nonlinear optical material for generating the second optical harmonic on the Nd: YAG laser (532 nm.

  1. 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

  2. Growth and Characterization of Tetraphenylphosphonium Bromide Crystal

    Directory of Open Access Journals (Sweden)

    Guangqiang Wang

    2017-05-01

    Full Text Available Multiple-phenyl phosphorous compounds are a group of chemical materials that have been used as reactants, pharmaceutical intermediates, extractants, and catalysts in organic synthetic reactions. However, the crystal growth of bulk crystals of multiple-phenyl phosphorous compounds, which may expand their applications in photonics technology, have been largely overlooked. In this article, the crystal growth of tetraphenylphosphonium bromide (TPPB has been studied in organic solvents and water. The crystal structures and crystallization features are analyzed by X-ray diffraction data. By a slow temperature-lowering method, a single-crystal of TPPB (2H2O with the size of 27 × 20 × 20 mm3 has been obtained in water. The basic thermal and optical properties were characterized. We find that the TPPB (2H2O crystal shows excellent transparent property in the near-IR region. Large Raman shifts and strong Raman scattering intensity indicate that TPPB is a potential candidate in Raman-scattering-based nonlinearity applications.

  3. High pressure studies of as grown WX2-x single crystals

    International Nuclear Information System (INIS)

    Solanki, G.K.; Agarwal, M.K.; Patel, Yogesh A.

    2011-01-01

    The structural optical and transport properties of tungsten metal dichalogenides having layered structure have been extensively studied in the last two decades. These materials shows highly anisotropic behaviour and have been receiving considerable interest for a variety of applications. Several of these layered semiconductors have attracted attention as a new class of solar cell material. We present here the results of simultaneous resistivity and thermoelectric power (TEP) measurements upto 7 GPa on single crystals of WS 2 , WS 1.9 , WSe 2 and WSe 1.9 grown using Direct Vapour Transport (DVT) technique. The observations clearly shows WS 2 and WS 1.9 are more resistive compared to other two crystals. In all samples an exponential fall of resistivity on increases in pressure upto 2.1 GPa but after 2.2 GPa the resistivity decreases substantially with increases pressure. The TEP of WSe 2 increases steadily and reaches maximum at 0.65 GPa, while for WSe 1.9 TEP increases upto pressure 0.5 GPa. In both the cases after attaining the maximum TEP, then decreases monotonically with increase in pressure. TEP of WS 2 and WS 1.9 increase upto pressure 1.1 GPa, beyond 1.1 GPa pressure in both the cases TEP decreases steadily with further increase in pressure. In all the samples, the sign of TEP is positive indicating that all of them are p-type and remain p-type with increase in pressure. The variation of thermoelectric power factor with pressure has been thoroughly studied. An analysis of the data point out that perfectly stoichiometric crystals of WSe 2 work as superior thermoelectric materials. The results have been presented and implications have been discussed. (author)

  4. Fractional decay of quantum dots in real photonic crystals

    DEFF Research Database (Denmark)

    Kristensen, Philip Trøst; Koenderink, A. Femius; Lodahl, Peter

    2008-01-01

    We show that fractional decay may be observable in experiments using quantum dots and photonic crystals with parameters that are currently achievable. We focus on the case of inverse opal photonic crystals and locate the position in the crystal where the effect is most pronounced. Furthermore, we...

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

    Science.gov (United States)

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

    2018-05-01

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

  6. Recurrent thermo-luminescence phenomenon in yttrium-aluminum garnet crystals

    International Nuclear Information System (INIS)

    Islamov, A.Kh.; Nuritdinov, I.; Esanov, Z.U.; Eshchanov, B.Kh.; Khayitov, I.A.

    2014-01-01

    Full text : The crystals of yttrium-aluminum garnet Y 2 Al 2 O 1 2 activated by cerium and praseodymium ions by their thermal and chemical durability as well as fast response are perspective scintillation materials. In this work the capture centres formed by action of the ionizing radiation on pure and doped by praseodymium and cerium crystals were investigated. The samples were grown using Chokhralsky method

  7. Growth and characterisation of lead iodide single crystals

    International Nuclear Information System (INIS)

    Tonn, Justus

    2012-01-01

    The work in hand deals with the growth and characterisation of lead iodide (PbI 2 ) single crystals. PbI 2 is regarded as a promising candidate for low-noise X- and gamma ray detection at room temperature. Its benefits if compared to conventional materials like HgI 2 , CdTe, Si, or GaAs lie in a band gap energy of 2.32 eV, an excellent ability to absorb radiation, and a high electrical resistivity. For an application of PbI 2 as detector material the growth and characterisation of crystals with high chemical and structural quality is extremely challenging. In light of this, the effectiveness of zone purification of the PbI 2 used for crystal growth was confirmed by spectroscopic analysis. Furthermore, technological aspects during processing of purified PbI 2 were investigated. With the help of thermal analysis, a correlation was found between the degree of exposing the source material to oxygen from the air and the structural quality of the resulting crystals. A hydrogen treatment was applied to PbI 2 as an effective method for the removal of oxidic pollutions, which resulted in a significant reduction of structural defects like polytypic growth and stress-induced cracking. The growth of PbI 2 single crystals was, among others, carried out by the Bridgman-Stockbarger method. In this context, much effort was put on the investigation of influences resulting from the design and preparation of ampoules. For the first time, crystal growth of PbI 2 was also carried out by the Czochralski method. If compared to the Bridgman-Stockbarger method, the Czochralski technique allowed a significantly faster growth of nearly crack-free crystals with a reproducible predetermination of crystallographic orientation. By an optimised sample preparation of PbI 2 , surface orientations perpendicular to the usually cleaved (0001) plane were realised. It is now possible to determine the material properties along directions which were so far not accessible. Thus, for example, the ratio of

  8. Effect of structural defects on the magnetic properties of the EuBaCo1.90O5.36 single crystal

    Science.gov (United States)

    Arbuzova, T. I.; Naumov, S. V.; Telegin, S. V.

    2018-01-01

    The effect of structural defects in cobalt and oxygen sublattices with the constant average oxidation level 3+ of all cobalt ions on the magnetic properties of the EuBaCo1.90O5.36 single crystal has been studied. The magnetic properties of the single crystal and the polycrystalline sample of the corresponding composition are compared in the range T = 200-650 K. The results show that the cobalt-deficient EuBaCo2- x O5.5-δ samples demonstrate a three-dimensional XY ferromagnetic ordering of magnetic sublattices. The values of the effective magnetic moment at T > 480 K indicate the existence of the IS and HS states of Co3+ ions. The large difference of values of μeff of the EuBaCo1.90O5.36 single crystal and polycrystal can be due to that the magnetic ion spins lie in plane ab. The magnetic field directed along plane ab substantially influences the magnetic ordering at T < 300 K.

  9. A study of the crystallization of ZrO

    International Nuclear Information System (INIS)

    Aguilar, D. H.; Torres-Gonzalez, L. C.; Torres-Martinez, L. M.; Lopez, T.; Quintana, P.

    2001-01-01

    ZrO(sub 2)-SiO(sub 2) sol-gel powders were produced using tetraethoxysilane (TEOS) and zirconium propoxide. After gellation, the ZrO(sub 2) crystallization process was investigated using X-ray diffraction (XRD), thermal analysis (DTA/TGA), and scanning electron microscopy (SEM). Fresh gels were amorphous. Thermal treatments were carried out from 100 to 1400 C for a total annealing time of 182 h. Tetragonal zirconia, (Z(t)) was the first phase to crystallize, between 300 and 500 C. Crystallization temperature was lower for zirconia-rich compositions, increasing as silica content was raised. DTA analysis showed that Z(t) crystallization occurred in two stages. Complete tetragonal-monoclinic zirconia transformation occurred near 1000 C, and was clearly observed only in ZrO(sub 2)-rich compositions ( and gt;80%). Silica remains amorphous until 1200 C, when ZrSiO(sub 4) formation took place. A metastable sol-gel phase diagram was proposed to show the crystallization process between 100 and 1400 C

  10. Linear, non-linear and thermal properties of single crystal of LHMHCl

    Science.gov (United States)

    Kulshrestha, Shobha; Shrivastava, A. K.

    2018-05-01

    The single crystal of amino acid of L-histidine monohydrochloride was grown by slow evaporation technique at room temperature. High optical quality and appropriate size of crystals were grown under optimized growth conditions. The grown crystals were transparent. Crystals are characterized with different characterizations such as Solubility test, UV-Visible, optical band gap (Eg). With the help of optical data to be calculate absorption coefficient (α), extinction coefficient (k), refractive index (n), dielectric constant (ɛ). These optical constants are shows favorable conditions for photonics devices. Second harmonic generation (NLO) test show the green light emission which is confirm that crystal have properties for laser application. Thermal stability of grown crystal is confirmed by TG/DTA.

  11. Early stage crystallization kinetics in metallic glass-forming alloys

    International Nuclear Information System (INIS)

    Louzguine-Luzgin, Dmitri V.

    2014-01-01

    Highlights: • Heterogeneous nucleation may precede the homogeneous one in an alloy. • High kinetic constants and the nucleation rate at the initial stage. • Metallic glasses have heterogeneous nucleation sites which saturate later. -- Abstract: The crystallization kinetics and structural changes of a few metallic glassy alloys were monitored using X-ray diffraction, transmission electron microscopy, differential scanning and isothermal calorimetry methods. Microstructural observations were used to estimate the nucleation and growth rates. A clear comparison of the differences in the crystallization kinetics in the metallic glassy samples is observed at the early and later crystallization stages

  12. Scanning near-field optical microscopy of quantum dots in photonic crystal cavities

    Energy Technology Data Exchange (ETDEWEB)

    Skacel, Matthias; Fiore, Andrea [COBRA Research Institute, Technical University Eindhoven, Den Dolech 2, 5600 MB Eindhoven (Netherlands); Prancardi, Marco; Gerardino, Annamaria [Institute of Photonics and Nanotechnology, CNR, via del Cineto Romano 42, 00156 Roma (Italy); Alloing, Blandine; Li Lianhe, E-mail: m.s.skacel@tue.n [Institute of Photonics and Quantum Electronics, EPFL, CH-1015 Lausanne (Switzerland)

    2010-09-01

    Nanophotonic devices are of major interest for research and future quantum communication applications. Due to their nanometer feature size the resolution limit of far-field microscopy poses a limitation on the characterization of their optical properties. A method to overcome the resolution limit is the Scanning Near-Field Optical Microscope (SNOM). By approaching a fiber tip into the close vicinity of the sample the optical emission in the near-field regime is collected. This way of collecting the light is not affected by the diffraction limit. We employ a low temperature SNOM to investigate the photoluminescence of InAs QDs emitting at 1300nm wavelength embedded in photonic crystal cavities. At each location of an image scan the tip is stopped and a spectrum is acquired. We then plot maps of the photoluminescence for each wavelength. With this instrument it is now possible to directly observe the coupling of QDs to photonic crystal cavities both spectrally and spatially. We show first results of photoluminescence mapping of InAs QDs in photonic crystal cavities.

  13. Crystallization and preliminary crystallographic analysis of merohedrally twinned crystals of MJ0729, a CBS-domain protein from Methanococcus jannaschii

    International Nuclear Information System (INIS)

    Fernández-Millán, Pablo; Kortazar, Danel; Lucas, María; Martínez-Chantar, María Luz; Astigarraga, Egoitz; Fernández, José Andrés; Sabas, Olatz; Albert, Armando; Mato, Jose M.; Martínez-Cruz, Luis Alfonso

    2008-01-01

    Trigonal crystals of MJ0729 showing different degrees of merohedral twinning that may vary from perfect hemihedral twinning to perfect tetartohedral twinning were obtained upon slight variation of the pH. CBS domains are small protein motifs, usually associated in tandem, that are implicated in binding to adenosyl groups. Several genetic diseases in humans have been associated with mutations in CBS sequences, which has made them very promising targets for rational drug design. Trigonal crystals of the CBS-domain protein MJ0729 from Methanococcus jannaschii were grown by the vapour-diffusion method at acidic pH. Preliminary analysis of nine X-ray diffraction data sets using Yeates statistics and Britton plots showed that slight variation in the pH as well as in the buffer used in the crystallization experiments led to crystals with different degrees of merohedral twinning that may vary from perfect hemihedral twinning to perfect tetartohedral twinning

  14. Effects of thermo-order-mechanical coupling on band structures in liquid crystal nematic elastomer porous phononic crystals.

    Science.gov (United States)

    Yang, Shuai; Liu, Ying

    2018-08-01

    Liquid crystal nematic elastomers are one kind of smart anisotropic and viscoelastic solids simultaneously combing the properties of rubber and liquid crystals, which is thermal sensitivity. In this paper, the wave dispersion in a liquid crystal nematic elastomer porous phononic crystal subjected to an external thermal stimulus is theoretically investigated. Firstly, an energy function is proposed to determine thermo-induced deformation in NE periodic structures. Based on this function, thermo-induced band variation in liquid crystal nematic elastomer porous phononic crystals is investigated in detail. The results show that when liquid crystal elastomer changes from nematic state to isotropic state due to the variation of the temperature, the absolute band gaps at different bands are opened or closed. There exists a threshold temperature above which the absolute band gaps are opened or closed. Larger porosity benefits the opening of the absolute band gaps. The deviation of director from the structural symmetry axis is advantageous for the absolute band gap opening in nematic state whist constrains the absolute band gap opening in isotropic state. The combination effect of temperature and director orientation provides an added degree of freedom in the intelligent tuning of the absolute band gaps in phononic crystals. Copyright © 2018 Elsevier B.V. All rights reserved.

  15. Compact TXRF system using doubly curved crystal optics

    International Nuclear Information System (INIS)

    Chen, Z.W.

    2000-01-01

    Doubly curved crystal optics can provide large collection solid angle from a small x-ray source but were difficult to be fabricated in the past. The recent innovative doubly curved crystal optic technology provides accurate bending figure of thin crystal and produces high performance doubly curved crystal optics. The high quality doubly curved crystal can increase the intensity of the primary beam significantly for total reflection x-ray fluorescence application based on a low power x-ray source. In this report, toroidal Si(220) crystals are used to focused Cu Kα and Mo Kα x-rays from low power compact x-ray tubes that have maximum power setting at 50 kV and 1 mA. With a slit aperture to control the convergent angle, a fan Cu Kα1 beam with 15 degree x 0.2 degree convergent angles is obtained for TXRF excitation. Similarly, a fan Mo Kα1 beam with 6 degree x 0.1 degree convergent angles is used for high energy excitation. Si wafer based TXRF samples will be prepared and measured using this technique and the experimental data. (author)

  16. Anti-solvent co-crystallization of carbamazepine and saccharin.

    Science.gov (United States)

    Wang, In-Chun; Lee, Min-Jeong; Sim, Sang-Jun; Kim, Woo-Sik; Chun, Nan-Hee; Choi, Guang J

    2013-06-25

    The co-crystal approach has been investigated extensively over the past decade as one of the most promising methods to enhance the dissolution properties of insoluble drug substances. Co-crystal powders are typically produced by mechanical grinding (neat or wet) or a solution method (evaporation or cooling). In this study, high-purity carbamazepine-saccharin (CBZ-SAC) co-crystals were manufactured by a novel method, anti-solvent addition. Among various solvents, methanol was found to perform well with water as the anti-solvent for the co-crystallization of CBZ and SAC. When water was added to the methanol solution of CBZ and SAC at room temperature under agitation, nucleation of CBZ-SAC co-crystals occurred within 2-3 min. Co-crystallization was complete after 30 min, giving a solid yield as high as 84.5% on a CBZ basis. The effects of initial concentrations, focusing on the SAC/CBZ ratio, were examined to establish optimal conditions. The whole anti-solvent co-crystallization process was monitored at-line via ATR-FTIR analysis of regularly sampled solutions. The nucleation and crystal growth of CBZ-SAC co-crystals were detected by a significant increase in absorption in the range of 2400-2260 cm(-1), associated with the formation of hydrogen bonds between the carbonyl group in CBZ and the N-H of SAC. When CBZ hydrates were formed as impurities during anti-solvent co-crystallization, the hydrogen bonding between methanol and water was reduced greatly, primarily due to the incorporation of water molecules into the CBZ crystal lattice. In conclusion, an anti-solvent approach can be used to produce highly pure CBZ-SAC co-crystal powders with a high solid yield. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Crystallization Kinetics of Barium and Strontium Aluminosilicate Glasses of Feldspar Composition

    Science.gov (United States)

    Hyatt, Mark J.; Bansal, Narottam P.

    1994-01-01

    Crystallization kinetics of BaO.Al2O3.2SiO2 (BAS) and SrO.Al2O3.2SiO2 (SAS) glasses in bulk and powder forms have been studied by non-isothermal differential scanning calorimetry (DSC). The crystal growth activation energies were evaluated to be 473 and 451 kJ/mol for bulk samples and 560 and 534 kJ/mol for powder specimens in BAS and SAS glasses, respectively. Development of crystalline phases on thermal treatments of glasses at various temperatures has been followed by powder x-ray diffraction. Powder samples crystallized at lower temperatures than the bulk and the crystallization temperature was lower for SAS glass than BAS. Crystallization in both glasses appeared to be surface nucleated. The high temperature phase hexacelsian, MAl2Si2O8 (M = Ba or Sr), crystallized first by nucleating preferentially on the glass surface. Also, monoclinic celsian does not nucleate directly in the glass, but is formed at higher temperatures from the transformation of the metastable hexagonal phase. In SAS the transformation to monoclinic celsian occurred rapidly after 1 h at 1100 C. In contrast, in BAS this transformation is sluggish and difficult and did not go to completion even after 10 h heat treatment at 1400 C. The crystal growth morphologies in the glasses have been observed by optical microscopy. Some of the physical properties of the two glasses are also reported.

  18. Dielectric and electro-optical parameters of two ferroelectric liquid crystals: a comparative study

    International Nuclear Information System (INIS)

    Kumar Misra, Abhishek; Kumar Srivastava, Abhishek; Shukla, J P; Manohar, Rajiv

    2008-01-01

    Dielectric relaxation and an electro-optical study of two ferroelectric liquid crystals having different spontaneous polarizations (Felix 16/100 and Felix 17/000) showing SmC* and SmA phases have been performed in the temperature range 30-80 compfn C. The experimental data have been used to determine different relaxation parameters, viz. distribution parameter, relaxation frequency, dielectric strength and rotational viscosity. The Goldstone mode of dielectric permittivity has been well observed for both the samples under investigation. The activation energy of both the samples has also been determined by the best theoretical fitting of the Arrhenius plot. We have also evaluated the optical response time and anchoring energy coefficients from electro-optical measurement techniques for these samples.

  19. The opto-thermal effect on encapsulated cholesteric liquid crystals

    Science.gov (United States)

    Liu, Yu-Sung; Lin, Hui-Chi; Yang, Kin-Min

    2017-12-01

    In this study, we implemented a micro-encapsulated CLC electronic paper that is optically addressed and electrically erasable. The mechanism that forms spot diameters on the CLC films is discussed and verified through various experimental parameters, including the thickness of CLCs and Poly(2,3-dihydrothieno-1,4-dioxin)-poly(styrenesulfonate) (PEDOT:PSS), pump intensity, and pumping time. The opto-thermal effect, brought on by the PEDOT:PSS absorbing layer, causes the spot diameters on the cholesteric liquid crystal thin films to vary. According to our results, the spot diameter is larger for a sample with a thinner cholesteric liquid crystal layer with the same excitation conditions and same thickness of the PEDOT layer. The spot diameter is also larger for a sample with a thicker PEDOT under the same excitation conditions and same thickness of the cholesteric liquid crystal layer. We proposed a simple heat-conducting model to explain the experimental results, which qualitatively agree with this theoretical model.

  20. Crystallization of Na2O-SiO2 gel and glass

    Science.gov (United States)

    Neilson, G. F.; Weinberg, M. C.

    1984-01-01

    The crystallization behavior of a 19 wt pct soda silica gel and gel-derived glass was compared to that of the ordinary glass of the same composition. Both bulk and ground glass samples were utilized. X-ray diffraction measurements were made to identify the crystalline phases and gauge the extent of crystallization. It was found that the gel crystallized in a distinctive manner, while the gel glass behavior was not qualitatively different from that of the ordinary glass.

  1. Synthesis, crystallization behavior and surface modification of Ni-Cr-Si-Fe amorphous alloy

    International Nuclear Information System (INIS)

    Iqbal, M.; Akhter, J.I.; Rajput, M.U.; Mahmood, K.; Hussain, Z.; Hussain, S.; Rafiq, M.

    2011-01-01

    A quaternary Ni/sub 86/Cr/sub 7/Si/sub 4/Fe/sub 3/ amorphous alloy was synthesized by melt spinning technique. Surface modification was done by electron beam melting (EBM), neutron irradiation and gamma-rays. Microstructure of as cast, annealed and modified samples was examined by scanning electron microscope. Crystallization behavior was studied by annealing the samples in vacuum at different temperatures in the range 773-1073 K. Techniques of X-ray diffraction (XRD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used for characterization. Differential scanning calorimetry (DSC) was conducted at various heating rates in the range 10-40 K/min. Thermal parameters like glass transition temperature T/sub g/, crystallization temperature T/sub x/, supercooled liquid region delta T/sub x/ and reduced glass transition temperature T/sub rg/ were measured. The Ni/sub 86/Cr/sub 7/Si/sub 4/Fe/sub 3/ alloy exhibits wide supercooled liquid region of 60 K indicating good thermal stability. The activation energy was calculated to be 160 +- 4 kJ/mol using Kissinger and Ozawa equations respectively which indicates high resistance against crystallization. The XRD results of the samples annealed at 773 K, 923 K, 973 K and 1073 K/20 min show nucleation of Ni/sub 2/Cr/sub 3/ and NiCrFe crystalline phases. Vickers microhardness of the as cast ribbon was measured to be 680. About 30-50 % increase in hardness was achieved by applying EBM technique. (author)

  2. Crystallization and melting behavior of poly(ethylene oxide) and its blend with styrene-based ionomer using time-resolved SAXS/WAXS experiments

    Energy Technology Data Exchange (ETDEWEB)

    Slusarczyk, CzesLaw, E-mail: cslusarczyk@ath.bielsko.pl [Institute of Textile Engineering and Polymer Materials, University of Bielsko-BiaLa, ul. Willowa 2, 43-309 Bielsko-BiaLa (Poland)

    2011-10-15

    Time-resolved synchrotron wide- and small-angle X-ray scattering experiments were used to investigate the crystallization behavior and microstructure development of neat poly(ethylene oxide) (PEO) and its 50/50 blend with ionomer containing 6.4 mol% of sodium acrylate. The apparent lateral crystal sizes D{sub (120)} and D{sub (112)/(004)} were derived from the WAXS profiles. It was found that D{sub (120)} and D{sub (112)/(004)} of PEO in the blend are almost independent of temperature and are smaller when compared to those of neat PEO sample. The evolution of morphological parameters extracted from time-resolved SAXS profiles such as the long period L, the lamellar crystal thickness l{sub C} and the amorphous layer thickness l{sub A}, shows that the crystallization process of neat PEO follows the nucleation theory. The lamellar crystal thickness l{sub C} shows a single linear dependence on inverse supercooling, over the whole temperature range investigated. In contrast, the crystallization process of PEO in the blend (i.e. in the presence of interactions with the ionomer) follows the nucleation theory only in the narrow supercooling range. It was found also that the morphology of the blend consists of a broad population of lamellar crystal thicknesses. During heating lamellae melt in the reversed sequence of their formation.

  3. Algorithms for solving atomic structures of nanodimensional clusters in single crystals based on X-ray and neutron diffuse scattering data

    International Nuclear Information System (INIS)

    Andrushevskii, N.M.; Shchedrin, B.M.; Simonov, V.I.

    2004-01-01

    New algorithms for solving the atomic structure of equivalent nanodimensional clusters of the same orientations randomly distributed over the initial single crystal (crystal matrix) have been suggested. A cluster is a compact group of substitutional, interstitial or other atoms displaced from their positions in the crystal matrix. The structure is solved based on X-ray or neutron diffuse scattering data obtained from such objects. The use of the mathematical apparatus of Fourier transformations of finite functions showed that the appropriate sampling of the intensities of continuous diffuse scattering allows one to synthesize multiperiodic difference Patterson functions that reveal the systems of the interatomic vectors of an individual cluster. The suggested algorithms are tested on a model one-dimensional structure

  4. Method for fitting crystal field parameters and the energy level fitting for Yb3+ in crystal SC2O3

    International Nuclear Information System (INIS)

    Qing-Li, Zhang; Kai-Jie, Ning; Jin, Xiao; Li-Hua, Ding; Wen-Long, Zhou; Wen-Peng, Liu; Shao-Tang, Yin; Hai-He, Jiang

    2010-01-01

    A method to compute the numerical derivative of eigenvalues of parameterized crystal field Hamiltonian matrix is given, based on the numerical derivatives the general iteration methods such as Levenberg–Marquardt, Newton method, and so on, can be used to solve crystal field parameters by fitting to experimental energy levels. With the numerical eigenvalue derivative, a detailed iteration algorithm to compute crystal field parameters by fitting experimental energy levels has also been described. This method is used to compute the crystal parameters of Yb 3+ in Sc 2 O 3 crystal, which is prepared by a co-precipitation method and whose structure was refined by Rietveld method. By fitting on the parameters of a simple overlap model of crystal field, the results show that the new method can fit the crystal field energy splitting with fast convergence and good stability. (condensed matter: electronic structure, electrical, magnetic, and optical properties)

  5. Virtual Crystallizer

    Energy Technology Data Exchange (ETDEWEB)

    Land, T A; Dylla-Spears, R; Thorsness, C B

    2006-08-29

    Large dihydrogen phosphate (KDP) crystals are grown in large crystallizers to provide raw material for the manufacture of optical components for large laser systems. It is a challenge to grow crystal with sufficient mass and geometric properties to allow large optical plates to be cut from them. In addition, KDP has long been the canonical solution crystal for study of growth processes. To assist in the production of the crystals and the understanding of crystal growth phenomena, analysis of growth habits of large KDP crystals has been studied, small scale kinetic experiments have been performed, mass transfer rates in model systems have been measured, and computational-fluid-mechanics tools have been used to develop an engineering model of the crystal growth process. The model has been tested by looking at its ability to simulate the growth of nine KDP boules that all weighed more than 200 kg.

  6. A multi-analyzer crystal spectrometer (MAX) for pulsed neutron sources

    International Nuclear Information System (INIS)

    Tajima, K.; Ishikawa, Y.; Kanai, K.; Windsor, C.G.; Tomiyoshi, S.

    1982-03-01

    The paper describes the principle and initial performance of a multi-analyzer crystal spectrometer (MAX) recently installed at the KENS spallation neutron source at Tsukuba. The spectrometer is able to make time of flight scans along a desired direction in reciprocal space, covering a wide range of the energy transfers corresponding to the fifteen analyzer crystals. The constant Q or constant E modes of operation can be performed. The spectrometer is particularly suited for studying collective excitations such as phonons and magnons to high energy transfers using single crystal samples. (author)

  7. Laser damage to production- and research-grade KDP crystals

    International Nuclear Information System (INIS)

    Rainer, F.; Atherton, L.J.; DeYoreo, J.J.

    1992-10-01

    We present the results of laser damage measurements conducted on potassium dihydrogen phosphate (KDP) and deuterated potassium dihydrogen phosphate (KD*P) crystals that were grown recently for both production and research applications by several sources. We have measured extrinsic damage thresholds that cover wavelengths from 1064 nm to 266 nm at pulse durations in the 3- to 10-ns regime. Many of the samples were extracted from boules grown specifically to yield large-area crystals, up to 32-cm square, for laser fusion applications. These crystals were the result of efforts, both by the Lawrence Livermore National Laboratory (LLNL) and commercial crystal-growth companies, to yield high-threshold KDP. In particular we have established that such crystals can reliably survive fluences exceeding 15 j/cm 2 at 355 nm and 20 j/cm 2 at 1064 nm when irradiated with 3-ns pulses. We present details of how bulk and surface damage to these crystals scale with pulse duration and wavelength as well as of morphological effects due to laser conditioning

  8. X-ray fluorescence holography studies for a Cu{sub 3}Au crystal

    Energy Technology Data Exchange (ETDEWEB)

    Dąbrowski, K.M., E-mail: karol.dabrowski@uj.edu.pl; Dul, D.T.; Jaworska-Gołąb, T.; Rysz, J.; Korecki, P.

    2015-12-01

    In this work we show that performing a numerical correction for beam attenuation and indirect excitation allows one to fully restore element sensitivity in the three-dimensional reconstruction of the atomic structure. This is exemplified by a comparison of atomic images reconstructed from holograms measured for ordered and disordered phases of a Cu{sub 3}Au crystal that clearly show sensitivity to changes in occupancy of the atomic sites. Moreover, the numerical correction, which is based on quantitative methods of X-ray fluorescence spectroscopy, was extended to take into account the influence of a disturbed overlayer in the sample.

  9. Thermo-electric oxidization of iron in lithium niobate crystals

    International Nuclear Information System (INIS)

    Falk, Matthias

    2007-01-01

    Lithium niobate crystals (LiNbO 3 ) are a promising material for nonlinear-optical applications like frequency conversion to generate visible light, e.g., in laser displays, but their achievable output power is greatly limited by the ''optical damage'', i.e., light-induced refractive-index changes caused by excitation of electrons from iron impurities and the subsequent retrapping in unilluminated areas of the crystal. The resulting space-charge fields modify the refractive indices due to the electro-optic effect. By this ''photorefractive effect'' the phase-matching condition, i.e., the avoidance of destructive interference between light generated at different crystal positions due to the dispersion of the fundamental wave and the converted wave, is disturbed critically above a certain light intensity threshold. The influence of annealing treatments conducted in the presence of an externally applied electric field (''thermo-electric oxidization'') on the valence state of iron impurities and thereby on the optical damage is investigated. It is observed that for highly iron-doped LiNbO 3 crystals this treatment leads to a nearly complete oxidization from Fe 2+ to Fe 3+ indicated by the disappearance of the absorption caused by Fe 2+ . During the treatment an absorption front forms that moves through the crystal. The absorption in the visible as well as the electrical conductivity are decreased by up to five orders of magnitude due to this novel treatment. The ratio of the Fe 2+ concentration to the total iron concentration - a measure for the strength of the oxidization - is in the order of 10 -6 for oxidized crystals whereas it is about 10 -1 for untreated samples. Birefringence changes are observed at the absorption front that are explained by the removal of hydrogen and lithium ions from the crystal that compensate for the charges of the also removed electrons from Fe 2+ . A microscopic shock-wave model is developed that explains the observed absorption front by

  10. 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.)

  11. Piezoelectric excitation of elastic waves in centrosymmetrical potassium tantalate crystal

    International Nuclear Information System (INIS)

    Smolenskij, G.A.; Lemanov, V.V.; Sotnikov, A.V.; Syrnikov, P.P.; Yushin, N.K.

    1981-01-01

    Experiment results on excitation of elastic oscillations in potassium tantalate crystals are considered. The experiment has been conducted by usual for supersonic measurements technique: an impulse of the variable electric field has been applied to one of plane-parallel sample end-faces, at the same end-face signals corresponding to elastic pulses propagating in the crystal have been detected. Basic radiopulses parameters: basic frequency 30 MHz, duration 1-2 μs, pulse recurrence frequency 500 Hz, power 10 W. The investigation carried out has shown that the application to the sample at T=80 K temperature of constant external electrical field parallel to direction of elastic wave propagation leads to hysteresis dependence of elastic waves amplitude on the external voltage value. With temperature increase the hysteresis loop is deformed. It has been found when investigating temperature dependence of elastic wave amplitude that in the absence of external constant electrical field in short-circuited by constant current samples the oxillation excitation effect disappears at T approximately equal to 200 K. An essential influence on the elastic wave amplitude value is exerted by illumination of the crystal surface by light with 360-630 nm wave length. At T 130 K bacaee of photovoltaic effect in illuminated samples [ru

  12. Strong crystal size effect on deformation twinning

    DEFF Research Database (Denmark)

    Yu, Qian; Shan, Zhi-Wei; Li, Ju

    2010-01-01

    plasticity. Accompanying the transition in deformation mechanism, the maximum flow stress of the submicrometre-sized pillars was observed to saturate at a value close to titanium’s ideal strength9, 10. We develop a ‘stimulated slip’ model to explain the strong size dependence of deformation twinning......Deformation twinning1, 2, 3, 4, 5, 6 in crystals is a highly coherent inelastic shearing process that controls the mechanical behaviour of many materials, but its origin and spatio-temporal features are shrouded in mystery. Using micro-compression and in situ nano-compression experiments, here we...... find that the stress required for deformation twinning increases drastically with decreasing sample size of a titanium alloy single crystal7, 8, until the sample size is reduced to one micrometre, below which the deformation twinning is entirely replaced by less correlated, ordinary dislocation...

  13. Effect of UV on the post irradiated Li Cs S O{sub 4} crystal by X and gamma radiation. Vol. 2

    Energy Technology Data Exchange (ETDEWEB)

    Kassem, M E [On Leave, Alexandria University, Faculty of Science, PHysics Department. Alexandria (Egypt); EL-Kolaly, M A [On Leave, Radiation Protection Department, Nuclear Research Center, Atomic Energy Authority, Cairo (Egypt); Al-Houty, L I [University of Qatar, Faculty of Science, Department of Physics, P.O. Box 2713, Doha (Qatar)

    1996-03-01

    Thermoluminescence characteristics of Li Cs S O{sub 4} crystal have been studied after exposure to different doses of X and Gamma-Radiations. The glow curves showed TL response of Three peaks at 75,125 and 250 degree C. The structure of the glow peaks due to X-rays is quite different from that due to gamma-rays. UV exposure yields regeneration of the TL peaks for the post irradiated samples with X or Gamma-radiation with some changes in the peaks`s structure especially the third peak. For the post X-ray irradiated crystals, the area under the third glow peak (PK III) increased with integrated time of UV exposure till about 30 min after which no changes were observed; while, for the post gamma-irradiated crystals, two linear regions were observed. The models of the TL response for the post irradiated samples as a result to UV are discussed. 5 figs.

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

    International Nuclear Information System (INIS)

    Razorenov, S. V.; Ivanchihina, G. E.; Kanel, G. I.; Herrmann, B.; Zaretsky, E. B.

    2007-01-01

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

  15. A more clear insight of the lysozyme crystal composition

    Energy Technology Data Exchange (ETDEWEB)

    Mueller, C.; Ulrich, J. [Martin-Luther-Universitaet Halle-Wittenberg, Zentrum fuer Ingenieurswissenschaften, Verfahrenstechnik/TVT, 06099 Halle Saale (Germany)

    2011-07-15

    Crystallization can be used as a purification method for proteins. Lysozyme was chosen as a model substance. Changing crystallization conditions will lead as shown to different lysozyme crystal morphologies with different properties. Beside others, lysozyme crystals can show a Tetragonal, High Temperature and Low Temperature Orthorhombic crystal morphology. Experiments such as conductivity measurements, pH tests, chloride detection tests, experiments using methylene blue as a dye and dissolution experiments were carried out to investigate the composition of the lysozyme crystals. It is proven that lysozyme crystals are made up of the initial buffer solution components: lysozyme (the protein), water which is part of the crystal lattice, salt ions which are attached to the protein molecule and voids filled with the buffer solution containing the crystallization agent (e.g. salt). Interesting dissolution behaviours of the lysozyme crystals were observed which are not described so far elsewhere (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  16. Lab-on-a-Chip Based Protein Crystallization

    Science.gov (United States)

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

    2001-01-01

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

  17. Research in garnet crystal (GSGG) development. Final report, 1 May 1984-31 December 1984

    International Nuclear Information System (INIS)

    Belt, R.F.; Uhrin, R.; Vemuri, K.

    1985-01-01

    This program describes the crystal growth of neodymium and chromium doped simultaneously into the host crystal of gadolinium scandium gallium garnet (Nd 3+ , Cr 3 +:Gd 3 (Sc,Ga) 2 Ga 3 O 12 or Nd,Cr:GSGG). Ten experimental boules were grown by the Czochralski method at a diameter of 1.0-1.2 inch. Special attention was given to congruently melting compositions, the Nd and Cr content, growth rate, atmosphere of growth, control of the solid liquid interface, and boule orientation. For each of our crystals a (0.25 x 3.00) inch cylindrical laser rod was extracted, fabricated, tested passively, and delivered to the Lawrence Livermore National Laboratory for active testing. At the same time, boule samples were examined for optical absorption, loss at 1.06μm, refractive index birefringence, and other physical properties. Results have demonstrated that optical quality can approach that of Nd:YAG in rod form. The increased efficiency of Nd,Cr:GSGG was confirmed to be about 2 times that of Nd:YAG. We also show that 2 inch diameter crystal boules can be grown successfully. It appears that larger boules are feasible for slab laser experiments

  18. Non-isothermal crystallization kinetics and characterization of biodegradable poly(butylene succinate-co-neopentyl glycol succinate) copolyesters

    International Nuclear Information System (INIS)

    Xie, Wen-Jie; Zhou, Xiao-Ming

    2015-01-01

    Both biodegradable aliphatic neat poly(butylene succinate) (PBS) and poly(butylene succinate-co-neopentyl glycol succinate) (P(BS-co-NPGS)) copolyesters with different 1,4-butanediol/neopentyl glycol ratios were synthesized through a two-step process of transesterification and polycondensation using stannous chloride and 4-Methylbenzenesulfonic acid as the co-catalysts. The structure, non-isothermal crystallization behavior, crystalline morphology and crystal structure of neat PBS and P(BS-co-NPGS) copolyesters were characterized by 1 H NMR, differential scanning calorimetry (DSC), polarized optical microscope (POM) and wide angle X-ray diffraction (WAXD), respectively. The Avrami equation modified by Jeziorny and Mo's method was employed to describe the non-isothermal crystallization kinetics of the neat PBS and its copolyesters. The modified Avrami equation could adequately describe the primary stage of non-isothermal crystallization kinetics of the neat PBS and its copolyesters. Mo's method provided a fairly satisfactory description of the non-isothermal crystallization of neat PBS and its copolyesters. Interestingly, the values of 1/t 1/2 , Z c and F(T) obtained by the modified Avrami equation and Mo's method analysis indicated that the crystallization rate increased first and then decreased with an increase of NPGS content compared that of neat PBS, whereas the crystallization mechanism almost kept unchanged. The results of tensile testing showed that the ductility of PBS was largely improved by incorporating NPGS units. The elongation at break increased remarkably with increasing NPGS content. In particular, the sample with 20% NPGS content showed around 548% elongation at break. - Highlights: • The incorporation of NPGS units reduced the spherulite size of BS unit. • The existence of NPGS units did not change the crystal structure of BS unit. • The NPGS units incorporated in PBS could significantly improve the ductility of PBS. • The

  19. Amine free crystal structure: The crystal structure of d(CGCGCG)2 and methylamine complex crystal

    International Nuclear Information System (INIS)

    Ohishi, Hirofumi; Tsukamoto, Koji; Hiyama, Yoichi; Maezaki, Naoyoshi; Tanaka, Tetsuaki; Ishida, Toshimasa

    2006-01-01

    We succeeded in the crystallization of d(CGCGCG) 2 and methylamine Complex. The crystal was clear and of sufficient size to collect the X-ray crystallographic data up to 1.0 A resolution using synchrotron radiation. As a result of X-ray crystallographic analysis of 2F o - F c map was much clear and easily traced. It is First time monoamine co-crystallizes with d(CGCGCG) 2 . However, methylamine was not found from the complex crystal of d(CGCGCG) 2 and methylamine. Five Mg ions were found around d(CGCGCG) 2 molecules. These Mg ions neutralized the anion of 10 values of the phosphate group of DNA with five Mg 2+ . DNA stabilized only by a metallic ion and there is no example of analyzing the X-ray crystal structure like this. Mg ion stabilizes the conformation of Z-DNA. To use monoamine for crystallization of DNA, we found that we can get only d(CGCGCG) 2 and Mg cation crystal. Only Mg cation can stabilize the conformation of Z-DNA. The method of using the monoamine for the crystallization of DNA can be applied to the crystallization of DNA of long chain of length in the future like this

  20. Design of Double PG Crystal Neutron Diffractometer

    International Nuclear Information System (INIS)

    Adib, M.; Habib, N.; El-Mesiry, M.S.; Fathallah, M.

    2011-01-01

    The design of a diffractometer containing two pyrolytic graphite (PG) crystals to select monochromatic neutrons in the range of wavelengths longer than 0.26 nm is given. The first crystal is high oriented pyrolytic graphite (HOPG) set at glancing angle to reflect monochromatic neutrons with a selected wavelength. The second is a low quality PG crystal filter, set at take-off-angle such that, it transmits the selected monochromatic neutrons and rejects the higher order contaminations accompanying the first order reflection. It was shown that, 2 mm thick of PG crystal having 0.30 FWHM on mosaic spread are the optimum parameters of monochromator PG crystal. While the optimum thickness and mosaic spread of the PG crystal filter were selected to have low contamination factor of higher order reflections. The optimum parameters of the PG filter crystal were calculated using the computer package Graphite recently developed in our laboratory. Calculation shows that, 3 cm thick PG filter (20 on mosaic spread) is sufficient to almost eliminate the higher order contaminations accompanying the main monochromatic neutrons with

  1. Crystal Growth Technology

    Science.gov (United States)

    Scheel, Hans J.; Fukuda, Tsuguo

    2004-06-01

    This volume deals with the technologies of crystal fabrication, of crystal machining, and of epilayer production and is the first book on industrial and scientific aspects of crystal and layer production. The major industrial crystals are treated: Si, GaAs, GaP, InP, CdTe, sapphire, oxide and halide scintillator crystals, crystals for optical, piezoelectric and microwave applications and more. Contains 29 contributions from leading crystal technologists covering the following topics: General aspects of crystal growth technology Silicon Compound semiconductors Oxides and halides Crystal machining Epitaxy and layer deposition Scientific and technological problems of production and machining of industrial crystals are discussed by top experts, most of them from the major growth industries and crystal growth centers. In addition, it will be useful for the users of crystals, for teachers and graduate students in materials sciences, in electronic and other functional materials, chemical and metallurgical engineering, micro-and optoelectronics including nanotechnology, mechanical engineering and precision-machining, microtechnology, and in solid-state sciences.

  2. Automated Sample Exchange Robots for the Structural Biology Beam Lines at the Photon Factory

    International Nuclear Information System (INIS)

    Hiraki, Masahiko; Watanabe, Shokei; Yamada, Yusuke; Matsugaki, Naohiro; Igarashi, Noriyuki; Gaponov, Yurii; Wakatsuki, Soichi

    2007-01-01

    We are now developing automated sample exchange robots for high-throughput protein crystallographic experiments for onsite use at synchrotron beam lines. It is part of the fully automated robotics systems being developed at the Photon Factory, for the purposes of protein crystallization, monitoring crystal growth, harvesting and freezing crystals, mounting the crystals inside a hutch and for data collection. We have already installed the sample exchange robots based on the SSRL automated mounting system at our insertion device beam lines BL-5A and AR-NW12A at the Photon Factory. In order to reduce the time required for sample exchange further, a prototype of a double-tonged system was developed. As a result of preliminary experiments with double-tonged robots, the sample exchange time was successfully reduced from 70 seconds to 10 seconds with the exception of the time required for pre-cooling and warming up the tongs

  3. Surface structures of normal paraffins and cyclohexane monolayers and thin crystals grown on the (111) crystal face of platinum. A low-energy electron diffraction study

    International Nuclear Information System (INIS)

    Firment, L.E.; Somorjai, G.A.

    1977-01-01

    The surfaces of the normal paraffins (C 3 --C 8 ) and cyclohexane have been studied using low-energy electron diffraction (LEED). The samples were prepared by vapor deposition on the (111) face of a platinum single crystal in ultrahigh vacuum, and were studied both as thick films and as adsorbed monolayers. These molecules form ordered monolayers on the clean metal surface in the temperature range 100--220 K and at a vapor flux corresponding to 10 -7 Torr. In the adsorbed monolayers of the normal paraffins (C 4 --C 8 ), the molecules lie with their chain axes parallel to the Pt surface and Pt[110]. The paraffin monolayer structures undergo order--disorder transitions as a function of temperature. Multilayers condensed upon the ordered monolayers maintained the same orientation and packing as found in the monolayers. The surface structures of the growing organic crystals do not corresond to planes in their reported bulk crystal structures and are evidence for epitaxial growth of pseudomorphic crystal forms. Multilayers of n-octane and n-heptane condensed upon disordered monolayers have also grown with the (001) plane of the triclinic bulk crystal structures parallel to the surface. n-Butane has three monolayer structures on Pt(111) and one of the three is maintained during growth of the crystal. Cyclohexane forms an ordered monolayer, upon which a multilayer of cyclohexane grows exhibiting the (001) surface orientation of the monoclinic bulk crystal structure. Surface structures of saturated hydrocarbons are found to be very susceptible to electron beam induced damage. Surface charging interferes with LEED only at sample thicknesses greater than 200 A

  4. Photorefractive lithium niobate crystals for applications in photonics

    International Nuclear Information System (INIS)

    Hartwig, U.

    2006-12-01

    Lithium niobate crystals (LiNbO 3 ) generally show a photorefractive response, i.e., light-induced refractive index changes. Crystals are investigated at room temperature and at elevated temperatures. As a result 'classical' photorefractive holographic volume-phase gratings, originating from space charge fields and the electro-optic effect, and 'non-classical' photorefractive volume-phase gratings, which can be traced back to strong absorption gratings, emerge. Single domain and periodically poled crystals (PPLN) are investigated. PPLN is typically used in non-linear optics for frequency conversion. The crystals also show non-linear photorefractive response during holographic recording with isotropically polarized light beams of equal intensity and, in the case of PPLN, by mixing of domain and holographic gratings. The results are important for applications combining the photorefractive and non-linear optical properties of LiNbO 3 . (orig.)

  5. Investigation of SiC crystals by means of synchrotron topography

    International Nuclear Information System (INIS)

    Wierzchowski, W.; Tymicki, E.; Balcer, T.; Pawlowska, M.; Wieteska, K.; Malinowska, A.; Wierzbicka, E.; Grasza, K.; Graeff, W.

    2006-01-01

    The crystallographic quality of monopolytypic 6H SiC crystals grown by Physical Vapour Transport in graphite crucible was studied. The diameter of crystals was increased up to 65 mm. The crystals were investigated using several methods of characterisation including white and monochromatic beam synchrotron diffraction topography and scanning electron microscopy. Particularly useful results were obtained using back reflection white beam synchrotron section topography, which provided the intersection of the large thickness of the sample investigated. The topographs revealed a great part of macro and micropipes present in the samples, reproduced as white areas. The additional possibility offered the section topographs taken using a fine grid with the distance between the wires equal to 0.7 mm, which enabled evaluation of the lattice deformation. The scanning electron microscopy was also very useful in studying the micropipes and voids as well as in observation of the selective etching pattern. (author)

  6. Monolayer atomic crystal molecular superlattices

    Science.gov (United States)

    Wang, Chen; He, Qiyuan; Halim, Udayabagya; Liu, Yuanyue; Zhu, Enbo; Lin, Zhaoyang; Xiao, Hai; Duan, Xidong; Feng, Ziying; Cheng, Rui; Weiss, Nathan O.; Ye, Guojun; Huang, Yun-Chiao; Wu, Hao; Cheng, Hung-Chieh; Shakir, Imran; Liao, Lei; Chen, Xianhui; Goddard, William A., III; Huang, Yu; Duan, Xiangfeng

    2018-03-01

    Artificial superlattices, based on van der Waals heterostructures of two-dimensional atomic crystals such as graphene or molybdenum disulfide, offer technological opportunities beyond the reach of existing materials. Typical strategies for creating such artificial superlattices rely on arduous layer-by-layer exfoliation and restacking, with limited yield and reproducibility. The bottom-up approach of using chemical-vapour deposition produces high-quality heterostructures but becomes increasingly difficult for high-order superlattices. The intercalation of selected two-dimensional atomic crystals with alkali metal ions offers an alternative way to superlattice structures, but these usually have poor stability and seriously altered electronic properties. Here we report an electrochemical molecular intercalation approach to a new class of stable superlattices in which monolayer atomic crystals alternate with molecular layers. Using black phosphorus as a model system, we show that intercalation with cetyl-trimethylammonium bromide produces monolayer phosphorene molecular superlattices in which the interlayer distance is more than double that in black phosphorus, effectively isolating the phosphorene monolayers. Electrical transport studies of transistors fabricated from the monolayer phosphorene molecular superlattice show an on/off current ratio exceeding 107, along with excellent mobility and superior stability. We further show that several different two-dimensional atomic crystals, such as molybdenum disulfide and tungsten diselenide, can be intercalated with quaternary ammonium molecules of varying sizes and symmetries to produce a broad class of superlattices with tailored molecular structures, interlayer distances, phase compositions, electronic and optical properties. These studies define a versatile material platform for fundamental studies and potential technological applications.

  7. Mesoscopic surface roughness of ice crystals pervasive across a wide range of ice crystal conditions

    Science.gov (United States)

    Magee, N. B.; Miller, A.; Amaral, M.; Cumiskey, A.

    2014-11-01

    Here we show high-magnification images of hexagonal ice crystals acquired by environmental scanning electron microscopy (ESEM). Most ice crystals were grown and sublimated in the water vapor environment of an FEI-Quanta-200 ESEM, but crystals grown in a laboratory diffusion chamber were also transferred intact and imaged via ESEM. All of these images display prominent mesoscopic topography including linear striations, ridges, islands, steps, peaks, pits, and crevasses; the roughness is not observed to be confined to prism facets. The observations represent the most highly magnified images of ice surfaces yet reported and expand the range of conditions in which rough surface features are known to be conspicuous. Microscale surface topography is seen to be ubiquitously present at temperatures ranging from -10 °C to -40 °C, in supersaturated and subsaturated conditions, on all crystal facets, and irrespective of substrate. Despite the constant presence of surface roughness, the patterns of roughness are observed to be dramatically different between growing and sublimating crystals, and transferred crystals also display qualitatively different patterns of roughness. Crystals are also demonstrated to sometimes exhibit inhibited growth in moderately supersaturated conditions following exposure to near-equilibrium conditions, a phenomenon interpreted as evidence of 2-D nucleation. New knowledge about the characteristics of these features could affect the fundamental understanding of ice surfaces and their physical parameterization in the context of satellite retrievals and cloud modeling. Links to supplemental videos of ice growth and sublimation are provided.

  8. Iron single crystal growth from a lithium-rich melt

    Science.gov (United States)

    Fix, M.; Schumann, H.; Jantz, S. G.; Breitner, F. A.; Leineweber, A.; Jesche, A.

    2018-03-01

    α -Fe single crystals of rhombic dodecahedral habit were grown from a Li84N12Fe∼3 melt. Crystals of several millimeter along a side form at temperatures around T ≈ 800 ° C. Upon further cooling the growth competes with the formation of Fe-doped Li3N. The b.c.c. structure and good sample quality of α -Fe single crystals were confirmed by X-ray and electron diffraction as well as magnetization measurements and chemical analysis. A nitrogen concentration of 90 ppm was detected by means of carrier gas hot extraction. Scanning electron microscopy did not reveal any sign of iron nitride precipitates.

  9. Nano Size Crystals of Geothite, alpha-FeOOH: Synthesis and Thermal Transformation

    Energy Technology Data Exchange (ETDEWEB)

    Christensen,A.; Jensen, T.; Bahl, C.; DiMasi, E.

    2007-01-01

    An aqueous suspension of amorphous iron(III) hydroxide was kept at room temperature (298 K) for 23 years. During this period of time the pH of the liquid phase changed from 4.3 to 2.85, and nano size crystals of goethite, {alpha}-FeOOH crystallized from the amorphous iron(III) hydroxide. Transmission electron microscopy (TEM) investigations, Moessbauer spectra, and powder X-ray diffraction using Co K{alpha} radiation showed that the only iron containing crystalline phase present in the recovered product was {alpha}-FeOOH. The size of these nano particles range from 10 to 100 nm measured by TEM. The thermal decomposition of {alpha}-FeOOH was investigated by time-resolved in situ synchrotron radiation powder X-ray diffraction and the data showed that the sample of {alpha}-FeOOH transformed to {alpha}-Fe{sub 2}O{sub 3} in the temperature range 444--584 K. A quantitative phase analysis shows the increase in scattered X-ray intensity from {alpha}-Fe{sub 2}O{sub 3} to follow the decrease of intensity from {alpha}-FeOOH in agreement with the topotactic phase transition.

  10. Crystallization and chemical durability of glasses in the system Bi2O3-SiO2

    International Nuclear Information System (INIS)

    Fredericci, C.

    2011-01-01

    The crystallization of the Bi 2 O 3 -SiO 2 -TiO 2 -Al 2 O 3 -Na 2 O-K 2 O and Bi 2 O 3 -SiO 2 -ZnO-Al 2 O 3 -B 2 O 3 -Na 2 O glasses was studied using glass samples prepared by traditional melt-quench method. Differential thermal analysis (DTA) curves suggested that surface crystallization played a major role in the crystallization of the glass samples. X-ray diffraction (XRD) analysis revealed the crystallization of bismuth silicate for both glasses and bismuth silicate and zinc silicate for the glass containing ZnO. Through scanning electron microscopy (MEV) and energy dispersive spectroscopy (EDS), it was possible to observe that the crystals of zinc silicate (Zn 2 SiO 4 ) were readily attacked by hot 0,1 N sulfuric acid, whereas bismuth silicate crystals were more resistant to acidic attack etching. (author)

  11. Effect of KrF excimer laser irradiation on the surface changes and photoelectric properties of ZnO single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Zeng, Yong [Institute of Laser Engineering, Beijing University of Technology, Beijing 100124 (China); Beijing Engineering Research Center of 3D Printing for Digital Medical Health, Beijing International Cooperation Base of 3D Printing for Digital MedicalHealth, Beijing University of Technology, Beijing 100124 (China); Zhao, Yan [Institute of Laser Engineering, Beijing University of Technology, Beijing 100124 (China); Jiang, Yijian, E-mail: yjjiang@bjut.edu.cn [Institute of Laser Engineering, Beijing University of Technology, Beijing 100124 (China); Beijing Engineering Research Center of 3D Printing for Digital Medical Health, Beijing International Cooperation Base of 3D Printing for Digital MedicalHealth, Beijing University of Technology, Beijing 100124 (China)

    2016-06-25

    In this paper, the effect of KrF pulsed excimer laser irradiation on the structural, surface morphology, photoluminescence and electrical properties of ZnO single crystal was investigated. Compared to the as-grown sample, at an irradiation energy density of 257 mJ/cm{sup 2}, the ZnO single crystal exhibits a series of phenomenon: XRD and Raman results show that the crystallization of ZnO quality change slightly, resistivity is decreased by two orders of magnitude, carrier concentration is increased by one order of magnitude. After laser irradiation, the surface shows some strip lines and no cracks. Formula calculation and simulation results show that the stripes are not caused by surface melting. We speculate that these stripes are caused by the precipitation of ZnO material inside to the surface. Due to the reduction of oxygen vacancies, UV emission has been enhanced and visible emission has been declined after irradiation. After the laser irradiation, the visible light of ZnO surface can be regulated. The experimental results show that KrF laser irradiation could effectively improve the optical and electrical properties of ZnO single crystal, which is important for the application of high performance of emitting optoelectronic devices. - Highlights: • After laser irradiation, the surface shows some strip lines and no cracks. • The visible light of as-irradiated ZnO surface can be regulated to four colors. • The electrical properties of as-irradiated ZnO has been improved greatly.

  12. Differentiation of organic and non-organic winter wheat cultivars from a controlled field trial by crystallization patterns.

    Science.gov (United States)

    Kahl, Johannes; Busscher, Nicolaas; Mergardt, Gaby; Mäder, Paul; Torp, Torfinn; Ploeger, Angelika

    2015-01-01

    There is a need for authentication tools in order to verify the existing certification system. Recently, markers for analytical authentication of organic products were evaluated. Herein, crystallization with additives was described as an interesting fingerprint approach which needs further evidence, based on a standardized method and well-documented sample origin. The fingerprint of wheat cultivars from a controlled field trial is generated from structure analysis variables of crystal patterns. Method performance was tested on factors such as crystallization chamber, day of experiment and region of interest of the patterns. Two different organic treatments and two different treatments of the non-organic regime can be grouped together in each of three consecutive seasons. When the k-nearest-neighbor classification method was applied, approximately 84% of Runal samples and 95% of Titlis samples were classified correctly into organic and non-organic origin using cross-validation. Crystallization with additive offers an interesting complementary fingerprint method for organic wheat samples. When the method is applied to winter wheat from the DOK trial, organic and non-organic treated samples can be differentiated significantly based on pattern recognition. Therefore crystallization with additives seems to be a promising tool in organic wheat authentication. © 2014 Society of Chemical Industry.

  13. Radiation of ultrarelativistic particles passing through ideal and mosaic crystals

    International Nuclear Information System (INIS)

    Afanas'ev, A.M.

    1977-01-01

    When a charged particle passes through an ideal crystal, then besides the transition radiation, a new kind of radiation, connected with the periodic structure of the crystal is produced. The influence of mosaic structure of a crystal on the intensity of this radiation is considered. Simple analytical expressions for the integral intensity of this radiation for the case of an ideal crystal are obtained. The results show, that the integral radiation intensity depends weakly on the degree of crystal perfection

  14. Growth of high-temperature superconductor crystals from flux

    International Nuclear Information System (INIS)

    Demianets, L.N.; Bykov, A.B.; Melnikov, O.K.; Stishov, S.M.

    1991-01-01

    Crystallization of high-temperature superconductors was studied in La-Sr-Cu-O, Y-Ba-Cu-O and Bi-Sr-Ca-Cu-O systems. Platelet crystals YBa 2 Cu 3 Osub(6.5+x) were obtained by spontaneous crystallization from homogeneous nonstoichiometric melts enriched in barium and copper oxides. Lasub(2-x)Sr x CuO 4 was prepared by slow cooling of melts enriched in copper oxide. Bi 2 (Sr, Ca)sub(n+1)Cu n O y , (n=1;2) was obtained by melting zone travelling. The crystals show transition to superconducting state at T=93K, ΔT 0.2-0.5 K (Y, Ba cuprate), T=87K, ΔT 2K (Bi, Sr, Ca-cuprate). La, Sr-cuprate single crystals obtained by Czochralski method did not show transition to superconducting state. For flux-grown crystals T c was 5-26 K depending on the composition, growth and heat treatment. The short characterization of some accessory phases (Ba 3 Y 2 Cu 3 PtO 10 , Casub(1.75)Srsub(1.5)Cusub(0.75)PtO 6 , BaCuO 2 , Ba 41 Cu 44 O 84 Cl 2 ) is reported. (author). 15 ref s., 8 figs

  15. A device for the application of uniaxial strain to single crystal samples for use in synchrotron radiation experiments

    Energy Technology Data Exchange (ETDEWEB)

    Gannon, L. [Clarendon Laboratory, University of Oxford Physics Department, Parks Road, Oxford OX1 3PU (United Kingdom); Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 ODE (United Kingdom); Bosak, A. [European Synchrotron Radiation Facility, BP 220, F-38043 Grenoble Cedex (France); Burkovsky, R. G. [European Synchrotron Radiation Facility, BP 220, F-38043 Grenoble Cedex (France); Peter the Great Saint-Petersburg Polytechnic University, 29 Politekhnicheskaya, 195251, St.-Petersburg (Russian Federation); Nisbet, G.; Hoesch, M., E-mail: Moritz.Hoesch@diamond.ac.uk [Diamond Light Source, Harwell Science and Innovation Campus, Didcot OX11 ODE (United Kingdom); Petrović, A. P. [DPMC-MaNEP, Université de Genève, Quai Ernest-Ansermet 24, 1211 Genève 4 (Switzerland)

    2015-10-15

    We present the design, construction, and testing of a straining device compatible with many different synchrotron radiation techniques, in a wide range of experimental environments (including low temperature, high field and ultra-high vacuum). The device has been tested by X-ray diffraction on single crystal samples of quasi-one-dimensional Cs{sub 2}Mo{sub 6}Se{sub 6} and K{sub 2}Mo{sub 6}Se{sub 6}, in which microscopic strains up to a Δc/c = 0.12% ± 0.01% change in the c lattice parameters have been achieved. We have also used the device in an inelastic X-ray scattering experiment, to probe the strain-dependent speed of sound ν along the c axis. A reduction Δν/ν of up to −3.8% was obtained at a strain of Δc/c = 0.25% in K{sub 2}Mo{sub 6}Se{sub 6}.

  16. Neutron beam applications - Development of single crystal structure analysis technique using the HANARO neutron four circle diffractometer

    Energy Technology Data Exchange (ETDEWEB)

    Suh, Il Hwan; Kim, Moon Jib; Kim, Jin Gyu [Chungnam National University, Taejon (Korea)

    2000-04-01

    As the four circle diffractometer (FCD) has been set up in HANARO, it has become possible to study the single crystal structures by means of the neutron diffraction. Taking account of the geometry of the FCD, a program for the control of te FCD and neutron data acquisition operating under Windows' circumstance has been accomplished. Also, a computer program which can automatically measure the diffraction intensity data has been developed. All data obtained from the FCD are processed automatically for further work and a software for the single crystal structure analyses has been prepared. A KC1 single crystal was selected as first test sample for a structure analysis had been successfully performed on the FCD using in-house developed program and accordingly their functionings with precision were confirmed. For regular single crystal diffraction experiments, the structure analyses of chrysoberyl and Zr(Y)0{sub 1.87} single crystals were performed using both neutron and X-ray diffraction methods, and the result showed that the neutron diffraction work is superior to the X-ray one from the viewpoint of certain crystallographic information obtainable only from the former one. 24 refs., 15 figs., 15 tabs. (Author)

  17. Principles of crystallization, and methods of single crystal growth

    International Nuclear Information System (INIS)

    Chacra, T.

    2010-01-01

    Most of single crystals (monocrystals), have distinguished optical, electrical, or magnetic properties, which make from single crystals, key elements in most of technical modern devices, as they may be used as lenses, Prisms, or grating sin optical devises, or Filters in X-Ray and spectrographic devices, or conductors and semiconductors in electronic, and computer industries. Furthermore, Single crystals are used in transducer devices. Moreover, they are indispensable elements in Laser and Maser emission technology.Crystal Growth Technology (CGT), has started, and developed in the international Universities and scientific institutions, aiming at some of single crystals, which may have significant properties and industrial applications, that can attract the attention of international crystal growth centers, to adopt the industrial production and marketing of such crystals. Unfortunately, Arab universities generally, and Syrian universities specifically, do not give even the minimum interest, to this field of Science.The purpose of this work is to attract the attention of Crystallographers, Physicists and Chemists in the Arab universities and research centers to the importance of crystal growth, and to work on, in the first stage to establish simple, uncomplicated laboratories for the growth of single crystal. Such laboratories can be supplied with equipment, which are partly available or can be manufactured in the local market. Many references (Articles, Papers, Diagrams, etc..) has been studied, to conclude the most important theoretical principles of Phase transitions,especially of crystallization. The conclusions of this study, are summarized in three Principles; Thermodynamic-, Morphologic-, and Kinetic-Principles. The study is completed by a brief description of the main single crystal growth methods with sketches, of equipment used in each method, which can be considered as primary designs for the equipment, of a new crystal growth laboratory. (author)

  18. Experimental evidence of infrared scintillation in crystals

    CERN Document Server

    Belogurov, S; Carugno, Giovanni; Conti, E; Iannuzzi, D; Meneguzzo, Anna Teresa

    2000-01-01

    We present experimental results on infrared emission induced by protons in some solid-state samples. Infrared scintillation occurs in many crystals, with different yield values and time-response behaviours. A rough measurement of the emission wavelength of CsI(Tl) is also reported.

  19. Liquid crystals: a new topic in physics for undergraduates

    International Nuclear Information System (INIS)

    Pavlin, Jerneja; Čepič, Mojca; Vaupotič, Nataša

    2013-01-01

    This paper presents a teaching module about liquid crystals. Since liquid crystals are linked to everyday student experiences and are also a topic of current scientific research, they are an excellent candidate for a modern topic to be introduced into education. We show that liquid crystals can provide a pathway through several fields of physics such as thermodynamics, optics and electromagnetism. We discuss what students should learn about liquid crystals and what physical concepts they should know before considering them. In the presentation of the teaching module, which consists of a lecture and experimental work in a chemistry and physics laboratory, we focus on experiments on phase transitions, polarization of light, double refraction and colours. A pilot evaluation of the module was performed among pre-service primary school teachers who have no special preference for natural sciences. The evaluation shows that the module is very efficient in transferring knowledge. A prior study showed that the informally obtained pre-knowledge on liquid crystals of the first-year students from several different fields of study was negligible. Since social science students are the least interested in natural sciences, it can be expected that students in any study programme will on average achieve at least as good qualitative knowledge of phenomena related to liquid crystals as the group involved in the pilot study. (paper)

  20. Inkjet printing of single-crystal films.

    Science.gov (United States)

    Minemawari, Hiromi; Yamada, Toshikazu; Matsui, Hiroyuki; Tsutsumi, Jun'ya; Haas, Simon; Chiba, Ryosuke; Kumai, Reiji; Hasegawa, Tatsuo

    2011-07-13

    The use of single crystals has been fundamental to the development of semiconductor microelectronics and solid-state science. Whether based on inorganic or organic materials, the devices that show the highest performance rely on single-crystal interfaces, with their nearly perfect translational symmetry and exceptionally high chemical purity. Attention has recently been focused on developing simple ways of producing electronic devices by means of printing technologies. 'Printed electronics' is being explored for the manufacture of large-area and flexible electronic devices by the patterned application of functional inks containing soluble or dispersed semiconducting materials. However, because of the strong self-organizing tendency of the deposited materials, the production of semiconducting thin films of high crystallinity (indispensable for realizing high carrier mobility) may be incompatible with conventional printing processes. Here we develop a method that combines the technique of antisolvent crystallization with inkjet printing to produce organic semiconducting thin films of high crystallinity. Specifically, we show that mixing fine droplets of an antisolvent and a solution of an active semiconducting component within a confined area on an amorphous substrate can trigger the controlled formation of exceptionally uniform single-crystal or polycrystalline thin films that grow at the liquid-air interfaces. Using this approach, we have printed single crystals of the organic semiconductor 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C(8)-BTBT) (ref. 15), yielding thin-film transistors with average carrier mobilities as high as 16.4 cm(2) V(-1) s(-1). This printing technique constitutes a major step towards the use of high-performance single-crystal semiconductor devices for large-area and flexible electronics applications.

  1. Amorphous photonic crystals with only short-range order.

    Science.gov (United States)

    Shi, Lei; Zhang, Yafeng; Dong, Biqin; Zhan, Tianrong; Liu, Xiaohan; Zi, Jian

    2013-10-04

    Distinct from conventional photonic crystals with both short- and long-range order, amorphous photonic crystals that possess only short-range order show interesting optical responses owing to their unique structural features. Amorphous photonic crystals exhibit unique light scattering and transport, which lead to a variety of interesting phenomena such as isotropic photonic bandgaps or pseudogaps, noniridescent structural colors, and light localization. Recent experimental and theoretical advances in the study of amorphous photonic crystals are summarized, focusing on their unique optical properties, artificial fabrication, bionspiration, and potential applications. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Improved success of sparse matrix protein crystallization screening with heterogeneous nucleating agents.

    Directory of Open Access Journals (Sweden)

    Anil S Thakur

    2007-10-01

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

  3. Annealing of KDP crystals in vacuum and under pressure

    International Nuclear Information System (INIS)

    Pritula, I.M.; Kolybayeva, M.I.; Salo, V.I.

    1997-01-01

    The effect of the high temperature annealing (T an > 230 degrees C) on the absorption spectra and laser damage threshold of KDP crystals was studied in the present paper. The experiments on isotermal annealing were performed under pressure in the atmosphere with specific properties. The composition of the atmosphere was selected to be chose to that of the desorbing gas component determined during annealing in vacuum. The mentioned conditions allowed to conduct annealing in the temperature range of 230 - 280 degrees C without degradation of the sample. The variations in the absorption spectra showed that the effect of the annealing is most strongly revealed in the short - wave region of the spectrum (λ -1 before and k=0.12 cm -1 after annealing) demonstrate that at temperatures ∼ 230 - 280 degrees C the processes ensuring the improvement of the structure quality are stimulated in the volume of the crystals: (a) before the annealing laser damage threshold was 1.5 10 11 W/cm 2 ; (b) after the annealing (t = 280 degrees C) it became 4 10 11 W/cm 2

  4. Room-temperature ferromagnetism observed in C-/N-/O-implanted MgO single crystals

    Science.gov (United States)

    Li, Qiang; Ye, Bonian; Hao, Yingping; Liu, Jiandang; Zhang, Jie; Zhang, Lijuan; Kong, Wei; Weng, Huimin; Ye, Bangjiao

    2013-01-01

    MgO single crystals were implanted with 70 keV C/N/O ions at room temperature with respective doses of 2 × 1016 and 2 × 1017 ions/cm2. All samples with high-dose implantation showed room temperature hysteresis in magnetization loops. Magnetization and slow positron annihilation measurements confirmed that room temperature ferromagnetism in O-implanted samples was attributed to the presence of Mg vacancies. Furthermore, the introduction of C or N played more effective role in ferromagnetic performance than Mg vacancies. Moreover, the magnetic moment possibly occurred from the localized wave function of unpaired electrons and the exchange interaction formed a long-range magnetic order.

  5. Initial testing of a Compact Crystal Positioning System for the TOPAZ Single-Crystal Diffractometer at the Spallation Neutron Source

    International Nuclear Information System (INIS)

    Frost, Matthew J.; Austin, Michael D.; Viola, Robert; Thomison, Jack; Carmen, Peter; Hoffmann, Christina; Miller, Echo M.; Mosier, Lisa B.; Overbay, Mark A.

    2009-01-01

    A precise, versatile, and automated method of orienting a sub-millimeter crystal in a focused neutron beam is required for e cient operation of the TOPAZ Single Crystal Di ractometer at the Spallation Neutron Source at Oak Ridge National Laboratory. To ful ll this need, a Compact Crystal Positioning System (CCPS) has been developed in collaboration with Square One Systems Design in Jackson, Wyoming. The system incorporates a tripod design with six vacuum-compatible piezoelectric linear motors capable of < 1 m resolution. National Instruments LabVIEW provides a means of system automation while at the same time accommodating the modular nature of the SNS sample environment control software for straightforward system integration. Initial results in a cryogenic test environment will be presented, as well as results from ambient tests performed at the Advanced Photon Source at Argonne National Laboratory.

  6. Nucleation and crystallization behaviors of nano-crystalline lithium–mica glass–ceramic prepared via sol–gel method

    Energy Technology Data Exchange (ETDEWEB)

    Tohidifar, M.R. [Department of Materials Science and Engineering, Tarbiat Modares University, P.O. Box 14115-143, Tehran (Iran, Islamic Republic of); Alizadeh, P., E-mail: p-alizadeh@modares.ac.ir [Department of Materials Science and Engineering, Tarbiat Modares University, P.O. Box 14115-143, Tehran (Iran, Islamic Republic of); Riello, P. [Department of Molecular Sciences and Nanosystems, University of Ca’Foscari, Venice (Italy)

    2012-06-15

    Graphical abstract: The effects of nucleation and crystallization treatments on nano-crystalline lithium–mica glass–ceramic, synthesized by sol–gel technique, were investigated. It was found that MgF{sub 2} crystals act as nuclei centers for the mica crystallization so that a large quantity of mica crystallites was obtained following nucleation process. The crystallization activation energy for both the un-nucleated and nucleated samples was measured as 400.2 and 229.6 kJ mol{sup −1}, respectively. The calculated Avrami exponents demonstrated that the growth mechanism of mica crystallites changes from the needle-like to three-dimensional growth with applying the appropriate nucleation treatment ▪. Highlights: ► Crystallization temperature shifts to 625 from 680 °C following nucleation process. ► Activation energy of crystallization for the nucleated specimen is 229.6 kJ mol{sup −1}. ► Crystallization activation energy for the un-nucleated specimen is 400.2 kJ mol{sup −1}. ► Needle-like growth is predominant growth mechanism for un-nucleated sample. ► Three-dimensional growth is predominant growth mechanism for nucleated sample. -- Abstract: The paper investigates the effects of nucleation and crystallization treatments on nano-crystalline lithium–mica glass–ceramics, taking the composition LiMg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6x}F{sub 2} (x = 0.5) and 8 mass% MgF{sub 2} synthesized by sol–gel technique. Here, X-ray diffraction, thermal analysis and transmission electron microscopy were used to assess the structural evolutions of as-synthesized nano-crystalline lithium–mica glass–ceramics. It was found that MgF{sub 2} crystals perform as nuclei centers for the mica crystallization hence; a large quantity of mica crystallites obtained following the nucleation process at 400 °C for 12 h. For both the un-nucleated and nucleated samples, the crystallization activation energy was measured as 400.2 and 229.6 kJ mol{sup −1

  7. Crystallization kinetics of magnetic glass-ceramics prepared by the processing of waste materials

    International Nuclear Information System (INIS)

    Francis, A.A.

    2006-01-01

    The objective of the present investigation was to study the feasibility of conversion of an intimate mixture of blast furnace slag and blast furnace flue dust generated by a single industrial company into magnetic glass-ceramic product. Blast furnace slag (BFS) and blast furnace flue dust (BFD) are generated at a rate of 300,000 and 30,000 tons/year, respectively, from iron and steel factory. The crystallization mechanisms of a composition containing BFS and BFD in a 50/50 proportion were investigated by differential thermal analysis (DTA), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The crystallization temperature was found to vary from 900 to 1100 deg. C and two phases appeared in the crystallized samples: pyroxene Ca(Mg, Fe, Al)(Si, Al) 2 O 6 and magnetite/maghemite. Heating rate and particle sizes effects on crystal growth of powdered samples were studied by DTA. The apparent activation energy of crystal growth using the particle size 180-315 μm was determined to be 355 and 329 kJ/mol for the first and second peak, respectively. The presence of sharp and broad crystallization peaks indicate simultaneous surface and internal crystallization mechanism. Good wear resistance and chemical durability particularly in alkaline environment, combine with good hardness and magnetic properties make this glass-ceramic material potentially useful for various industrial applications

  8. Ge-Au eutectic bonding of Ge (100) single crystals

    International Nuclear Information System (INIS)

    Knowlton, W.B.; Beeman, J.W.; Emes, J.H.; Loretto, D.; Itoh, K.M.; Haller, E.E.

    1993-01-01

    The author present preliminary results on the eutectic bonding between two (100) Ge single crystal surfaces using thin films of Au ranging from 900 angstrom/surface to 300 angstrom/surface and Pd (10% the thickness of Au). Following bonding, plan view optical microscopy (OM) of the cleaved interface of samples with Au thicknesses ≤ 500 angstrom/surface show a eutectic morphology more conducive to phonon transmission through the bond interface. High resolution transmission electron microscopy (HRTEM) cross sectional interface studies of a 300 angstrom/surface Au sample show epitaxial growth of Ge. In sections of the bond, lattice continuity of the Ge is apparent through the interface. TEM studies also reveal heteroepitaxial growth of Au with a Au-Ge lattice mismatch of less than 2%. Eutectic bonds with 200 angstrom/surface Au have been attained with characterization pending. An optical polishing technique for Ge has been optimized to insure intimate contact between the Ge surfaces prior to bonding. Interferometry analysis of the optically polished Ge surface shows that surface height fluctuations lie within ±150 angstrom across an interval of lmm. Characterization of phonon transmission through the interface is discussed with respect to low temperature detection of ballistic phonons

  9. Tensometrical properties of volumetric crystals of germanium-silicon solid solutions irradiated by fast electrons

    International Nuclear Information System (INIS)

    Abbasov, Sh.M.

    2002-01-01

    Full Text: In the present work the tensometrical properties of Ge1-xSix solid solution monocrystal contended of up to 15 at. % Si were investigated. The radiation-proof strain gauges of researched crystals were made. For this purpose the site was cutted out from a sample, perpendicularly or in parallel of a crystal axes. After polishing the samples had thickness of 30-40 microns, and length of 2 mm

  10. Resistive switching behavior in single crystal SrTiO{sub 3} annealed by laser

    Energy Technology Data Exchange (ETDEWEB)

    Pan, Xinqiang [State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Shuai, Yao, E-mail: yshuai@uestc.edu.cn [State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Collaboration Innovation Center of Electronic Materials and Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Wu, Chuangui, E-mail: cgwu@uestc.edu.cn [State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Collaboration Innovation Center of Electronic Materials and Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Luo, Wenbo [State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Collaboration Innovation Center of Electronic Materials and Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Sun, Xiangyu [State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Yuan, Ye; Zhou, Shengqiang [Helmholtz-Zentrum Dresden Rossendorf, Institute of Ion Beam Physics and Materials Research, Bautzner Landstrasse 400, D-01328 Dresden (Germany); Ou, Xin [State Key Laboratory of Functional Material for Informatics, Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences, Shanghai 200050 (China); Zhang, Wanli [State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China); Collaboration Innovation Center of Electronic Materials and Devices, University of Electronic Science and Technology of China, Chengdu 610054 (China)

    2016-12-15

    Highlights: • Laser annealing was used to introduce oxygen vacancies into the single crystal SrTiO{sub 3}. • The effect of laser annealing with different fluence on the single crystal SrTiO{sub 3} was systematically studied. • The concentration of oxygen vacancies can be tuned by changing the fluence of laser. • Resistive switching behavior was observed in the sample with relatively high laser fluence after an electro-forming process. - Abstract: Single crystal SrTiO{sub 3} (STO) wafers were annealed by XeCl laser (λ = 308 nm) with different fluences of 0.4 J/cm{sup 2}, 0.6 J/cm{sup 2} and 0.8 J/cm{sup 2}, respectively. Ti/Pt electrodes were sputtered on the surface of STO wafer to form co-planar capacitor-like structures of Pt/Ti/STO/Ti/Pt. Current-Voltage measurements show that the leakage current is enhanced by increasing laser fluence. Resistive switching behavior is only observed in the sample annealed by laser with relatively high fluence after an electro-forming process. The X-ray photoelectron spectroscopy measurements indicate that the amount of oxygen vacancies increases with the increase of laser fluence. This work indicates resistive switching appears when enough oxygen vacancies are generated by the laser, which form conductive filaments under an external electric field.

  11. The melting and crystallization behavior of irradiated poly(1-butene)

    International Nuclear Information System (INIS)

    Markovic, V.; Silverman, J.

    1982-01-01

    Isotactic poly(1-butene) samples were melted and crystallized. This treatment leaves the polymer in the unstable crystalline form, known as Modification II. The transformation to stable Modification I normally has a half life of 1 day. Samples were irradiated within 30 min after crystallization with high doses of electrons delivered in intervals up to a few minutes. This permitted measurements of radiation effects on Modification II under circumstances where the II-I crystal transformation was negligibly small. Similar measurements were performed on stable Modification I, which was obtained by waiting for the completion of the II-I transformation; for this stable crystalline form, relatively low dose rate γ-exposures serve as well as high dose rate electron beams in measuring radiation effects. DSC and IR absorption measurements were performed. The effect of radiation on the fusion endotherms, melting points, IR spectra, and some aspects of the kinetics of crystalline transformation are presented. (author)

  12. Preparation and photonic bandgap properties of Na1/2Bi1/2TiO3 inverse opal photonic crystals

    International Nuclear Information System (INIS)

    Yang Zhengwen; Zhou Ji; Huang Xueguang; Xie Qin; Fu Ming; Li Bo; Li Longtu

    2009-01-01

    The Na 1/2 Bi 1/2 TiO 3 (NBT) inverse opal photonic crystals were prepared by the self-assembly technique in combination with a sol-gel method. In the preparation process, NBT precursors were filled into the interstices of the opal template assembled by monodispersive polystyrene microspheres. The polystyrene template was then removed by calcination at 800 deg. C for 5 h, meanwhile, a perovskite NBT inverse opal photonic crystal was formed. An optical micrograph shows that the NBT inverse opals reflect green-yellow light strongly. Moreover, a photonic band gap was observed by reflective spectra of NBT sample

  13. Study on the crystallization of multiarm stars with a poly(ethyleneimine) core and poly(ϵ-caprolactone) arms of different length

    Energy Technology Data Exchange (ETDEWEB)

    Díaz, Angélica; Bacaicoa, Anna; Casas, Maria Teresa; Franco, Lourdes [Departament d’Enginyeria Química, Universitat Politècnica de Catalunya, Av. Diagonal 647, Barcelona E-08028 (Spain); Serra, Angels [Departament de Química Analítica i Química Orgànica, Universitat Rovira i Virgili. C. Marcel.lí Domingo, s/n. Campus Sescelades, Tarragona 43007 (Spain); Puiggalí, Jordi, E-mail: Jordi.Puiggali@upc.edu [Departament d’Enginyeria Química, Universitat Politècnica de Catalunya, Av. Diagonal 647, Barcelona E-08028 (Spain)

    2015-05-10

    Highlights: • Isothermal crystallization kinetics of multiarm stars. • Influence of the length of poly(ϵ-caprolactone) arms on crystallization kinetics. • Influence of the length of poly(ϵ-caprolactone) arms on secondary nucleation constant. • Crystallization of mixtures of stars having different arm lengths. - Abstract: Crystallization of multiarm star systems constituted by a core of poly(ethyleneimine) (PEI) and arms of poly(ϵ-caprolactone) (PCL) was studied by transmission electron microscopy, calorimetry and optical microscopy techniques. Three systems differing on the degree of polymerization of PCL were studied as well as binary mixtures constituted by systems differing on the length of PCL arms. Samples were able to crystallize from both diluted solutions and the melt state giving rise to well-formed lamellae and spherulites, respectively. Lamellae of samples with large PCL arms were highly regular and corresponded to elongated hexagonal crystals with an aspect ratio that decreased with the length of PCL arms. A significant decrease on equilibrium melting temperatures, degree of crystallinity and glass transition temperature was detected for samples having short PCL arms. Crystallization kinetics were also highly influenced by the length of PCL arms, being both nucleation density and secondary nucleation constant increased as the length of PCL arms decreased. Crystallization of star mixtures having different PCL lengths was determined by the larger arms since they initiated the process and subsequently shorter arms were progressively incorporated. A thermal nucleation was characteristic of multiarm star mixtures due to the different crystallization temperature ranges of samples with large and short PCL arms, whereas samples with a homogeneous arm length rendered an athermal nucleation.

  14. Crystal growth and scintillation properties of Pr-doped oxyorthosilicate for different concentration

    Energy Technology Data Exchange (ETDEWEB)

    Totsuka, Daisuke, E-mail: totsuka@mail.tagen.tohoku.ac.jp [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); Nihon Kessho Kogaku Co. Ltd (Japan); Yanagida, Takayuki [New Industry Creation Hatchery Center (NICHe) 6-6-10 Aoba, Aramaki, Aoba-ku, Sendai, Miyagi 980-8579 (Japan); Fujimoto, Yutaka [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); Pejchal, Jan [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); Institute of Physics AS CR, Cukrovarnicka 10, Prague 6, 162-53 (Czech Republic); Yokota, Yuui [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); Yoshikawa, Akira [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); New Industry Creation Hatchery Center (NICHe) 6-6-10 Aoba, Aramaki, Aoba-ku, Sendai, Miyagi 980-8579 (Japan)

    2011-07-01

    0.05, 0.1 and 0.25 mol% Pr (with respect to Lu) doped Lu{sub 2}SiO{sub 5} (LSO) single crystals were grown by the micro-pulling down ({mu}-PD) method. The grown crystals were transparent, and a slight segregation of Pr{sup 3+} was observed both in the crystal cross-section and growth direction. Transparency in the visible wavelength range was about 80% in all the crystals. Intense absorptions related with the Pr{sup 3+} 4f-5d transitions were observed around 230 and 255 nm, and weak absorptions due to the 4f-4f transitions were detected around 450 nm. In radioluminescence spectra, the Pr{sup 3+} 5d-4f transitions were observed around 275and 310 nm, and emissions due to the 4f-4f transition were observed around 500 nm. In the pulse height analysis using {sup 137}Cs gamma-ray excitation, Pr 0.1% doped sample showed the highest light yield of 2,800 ph/MeV. In the decay time measurements using different excitation sources (photoluminescence, X- and gamma-ray), two different processes related to the 5d-4f emission peaks were found. Fast decay component corresponds to direct excitation of Pr{sup 3+} (4-6 ns) and slower component (25 ns) reflects the energy migration process from the host lattice to the emission center.

  15. Electrically modulated transparent liquid crystal-optical grating projection

    DEFF Research Database (Denmark)

    Buss, Thomas; Smith, Cameron; Kristensen, Anders

    2013-01-01

    A transparent, fully integrated electrically modulated projection technique is presented based on light guiding through a thin liquid crystal layer covering sub-wavelength gratings. The reported device operates at 10 V with response times of 4.5 ms. Analysis of the liquid crystal alignment shows...

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

    Science.gov (United States)

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

    2017-12-01

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

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

    Science.gov (United States)

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

    2013-09-03

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

  18. The Taylor relation in compression deformed Ge single crystals

    International Nuclear Information System (INIS)

    Nyilas, K; Ungar, T; Dupas, C; Martin, J L; Kruml, T

    2010-01-01

    Ge single crystals are deformed in compression at 850K and the same strain rate to various extents of strains. In each sample, the internal stress is measured through stress reduction tests and the dislocation densities by X-ray measurements. Data about these two parameters follow fairly well the Taylor-Saada relation, provided a correction term is added. It probably corresponds to dislocations which are seen by X-rays, though they do not contribute to crystal hardening.

  19. Perturbed angular correlation study of surface magnetization in iron single crystals

    International Nuclear Information System (INIS)

    Sawicka, B.D.; Sawicki, J.A.; Pleiter, F.; Waard, H. de

    1983-01-01

    The behaviour of closure domains at the surface of iron single crystals in an external magnetic field was studied by DPAC on samples implanted with 111 In. It is observed that the surface magnetization does not follow that of the bulk. The movement of both the 90 0 and 180 0 walls of the closure domains is blocked up to a certain 'starting' value of the external field that is related to the demagnetization factor of the sample and also depends on the precise orientation of the crystal axes and on the implanted indium dose. (Auth.)

  20. Band structures of two dimensional solid/air hierarchical phononic crystals

    International Nuclear Information System (INIS)

    Xu, Y.L.; Tian, X.G.; Chen, C.Q.

    2012-01-01

    The hierarchical phononic crystals to be considered show a two-order “hierarchical” feature, which consists of square array arranged macroscopic periodic unit cells with each unit cell itself including four sub-units. Propagation of acoustic wave in such two dimensional solid/air phononic crystals is investigated by the finite element method (FEM) with the Bloch theory. Their band structure, wave filtering property, and the physical mechanism responsible for the broadened band gap are explored. The corresponding ordinary phononic crystal without hierarchical feature is used for comparison. Obtained results show that the solid/air hierarchical phononic crystals possess tunable outstanding band gap features, which are favorable for applications such as sound insulation and vibration attenuation.

  1. Band structures of two dimensional solid/air hierarchical phononic crystals

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Y.L.; Tian, X.G. [State Key Laboratory for Mechanical Structure Strength and Vibration, Xi' an Jiaotong University, Xi' an 710049 (China); Chen, C.Q., E-mail: chencq@tsinghua.edu.cn [Department of Engineering Mechanics, AML and CNMM, Tsinghua University, Beijing 100084 (China)

    2012-06-15

    The hierarchical phononic crystals to be considered show a two-order 'hierarchical' feature, which consists of square array arranged macroscopic periodic unit cells with each unit cell itself including four sub-units. Propagation of acoustic wave in such two dimensional solid/air phononic crystals is investigated by the finite element method (FEM) with the Bloch theory. Their band structure, wave filtering property, and the physical mechanism responsible for the broadened band gap are explored. The corresponding ordinary phononic crystal without hierarchical feature is used for comparison. Obtained results show that the solid/air hierarchical phononic crystals possess tunable outstanding band gap features, which are favorable for applications such as sound insulation and vibration attenuation.

  2. Structure, spectra and phase transition in p-nitroanilinium perchlorate crystal

    Energy Technology Data Exchange (ETDEWEB)

    Marchewka, M.K.; Drozd, M.; Pietraszko, A

    2003-07-25

    The first X-ray diffraction and vibrational spectroscopic analysis of a novel complex between p-nitroaniline and perchloric acid is reported. The structure was solved in 295 K. Room temperature powder infrared and Raman measurements for the p-nitroanilinium perchlorate (1:1) crystals were carried out. The vibrational spectra in the region of internal vibrations of ions corroborates the X-ray data which show that p-nitroaniline molecule is monoprotonated. DSC measurements on powder sample indicate the phase transition point at about 213 and 208 K for heating and cooling, respectively. No detectable signal was observed during powder test for second harmonic generation.

  3. Thermoluminescence and F centers of manganese doped NaCl and NaCl-CKl crystals exposed to gamma radiation

    International Nuclear Information System (INIS)

    Somera, L.; Cruz Z, E.; Roman L, J.; Hernandez A, J. M.; Murrieta S, H.

    2015-10-01

    Alkali halides crystals doped with rare earths or transition metals have been widely studied due to the luminescence properties. In particular, NaCl and KCl single crystals present thermally stimulated luminescence (Tl) after gamma irradiation. The NaCl and the NaCl KCl mixed crystal doped with manganese (MnCl 2 ) impurity were grown by using the Czochralski method. The emission characteristic of Mn 2+ was observed at 543 nm. The crystals were exposed between 0.02 and 10 kGy gamma dose from 60 Co irradiator. Optical absorption at room temperature shows the peaked band at 452 nm corresponding to the manganese impurity. The F bands, was ascribed to the electron trapped in the anion vacancy in the lattice, were obtained at 452 nm and 455 nm belonging to NaCl:Mn and NaCl KCl:Mn, respectively. The F band increases as the doses increase and it was bleaching by the UV light at 470 nm. The glow curves of the samples show the first glow peak between 92-103 degrees C, while the second main peak was observed at 183 degrees C for the undoped NaCl and at 148 and 165 degrees C for the NaCl:Mn and NaCl-KCl:Mn, respectively. The main peak was slowly bleaching when the irradiated sample was illuminated with F (470 nm) light. Optical bleaching confirms that the F center has an important participation in the thermoluminescent response. The glow curves structure from the thermal bleaching suggests the participation of different kind of traps. Also, the kinetics parameters such as activation energy (E), frequency factor (s) and the kinetic order (b) were investigated. (Author)

  4. Thermoluminescence and F centers of manganese doped NaCl and NaCl-CKl crystals exposed to gamma radiation

    Energy Technology Data Exchange (ETDEWEB)

    Somera, L.; Cruz Z, E.; Roman L, J. [UNAM, Instituto de Ciencias Nucleares, Circuito Exterior, Ciudad Universitaria, 04510 Mexico D. F. (Mexico); Hernandez A, J. M.; Murrieta S, H., E-mail: ecruz@nucleares.unam.mx [UNAM, Instituto de Fisica, Circuito Exterior, Ciudad Universitaria, 04510 Mexico D. F. (Mexico)

    2015-10-15

    Alkali halides crystals doped with rare earths or transition metals have been widely studied due to the luminescence properties. In particular, NaCl and KCl single crystals present thermally stimulated luminescence (Tl) after gamma irradiation. The NaCl and the NaCl KCl mixed crystal doped with manganese (MnCl{sub 2}) impurity were grown by using the Czochralski method. The emission characteristic of Mn{sup 2+} was observed at 543 nm. The crystals were exposed between 0.02 and 10 kGy gamma dose from {sup 60}Co irradiator. Optical absorption at room temperature shows the peaked band at 452 nm corresponding to the manganese impurity. The F bands, was ascribed to the electron trapped in the anion vacancy in the lattice, were obtained at 452 nm and 455 nm belonging to NaCl:Mn and NaCl KCl:Mn, respectively. The F band increases as the doses increase and it was bleaching by the UV light at 470 nm. The glow curves of the samples show the first glow peak between 92-103 degrees C, while the second main peak was observed at 183 degrees C for the undoped NaCl and at 148 and 165 degrees C for the NaCl:Mn and NaCl-KCl:Mn, respectively. The main peak was slowly bleaching when the irradiated sample was illuminated with F (470 nm) light. Optical bleaching confirms that the F center has an important participation in the thermoluminescent response. The glow curves structure from the thermal bleaching suggests the participation of different kind of traps. Also, the kinetics parameters such as activation energy (E), frequency factor (s) and the kinetic order (b) were investigated. (Author)

  5. Metal-loaded pollucite-like aluminophosphates: dissymmetrisation of crystal structures and physical properties

    Science.gov (United States)

    Shvanskaya, L. V.; Yakubovich, O. V.; Koshelev, A. V.; Vasiliev, A. N.

    2018-02-01

    Two aluminophosphate analogues of the mineral pollucite with the general formula Cs2(M,Al)3P3O12 (where M = Cu or Mn) have been synthesized by high-temperature flux and structurally characterized using the single-crystal X-ray diffraction. Both samples crystallize in cubic I4132 space group, Z = 8, with a = 13.5911(5) and a = 13.8544(7) for Cu- and Mn-loaded phases, respectively. Their framework structures are based on the ANA-type topology and exhibit the partial ordering of the metal (M/Al) and phosphorus (P) cations over the tetrahedral sites. The regular changes in cell dimensions and volumes in the row Cs2(Cu,Al)3P3O12→Cs2(Mn,Al)3P3O12 obviously correspond to increasing radii of the transition metal. The crystal chemical analysis of both pollucite-like phases show correlations between the difference in the radii size of tetrahedral cations and the degree of distortion of flexible ANA-type framework due to decreasing of the intertetrahedral angles (T-O-T). Magnetic susceptibility measurements indicate that both compounds are paramagnets in the temperature range of 2-300 K.

  6. Experimental study on the sound absorption characteristics of continuously graded phononic crystals

    Directory of Open Access Journals (Sweden)

    X. H. Zhang

    2016-10-01

    Full Text Available Novel three-dimensional (3D continuously graded phononic crystals (CGPCs have been designed, and fabricated by 3D printing. Each of the CGPCs is an entity instead of a combination of several other samples, and the porosity distribution of the CGPC along the incident direction is nearly linear. The sound absorption characteristics of CGPCs were experimentally investigated and compared with those of uniform phononic crystals (UPCs and discretely stepped phononic crystals (DSPCs. Experimental results show that CGPCs demonstrate excellent sound absorption performance because of their continuously graded structures. CGPCs have higher sound absorption coefficients in the large frequency range and more sound absorption coefficient peaks in a specific frequency range than UPCs and DSPCs. In particular, the sound absorption coefficients of the CGPC with a porosity of 0.6 and thickness of 30 mm are higher than 0.56 when the frequency is 1350–6300 Hz and are all higher than 0.2 in the studied frequency range (1000–6300 Hz. CGPCs are expected to have potential application in noise control, especially in the broad frequency and low-frequency ranges.

  7. Distributions of crystals and gas bubbles in reservoir ice during growth period

    Directory of Open Access Journals (Sweden)

    Zhi-jun Li

    2011-06-01

    Full Text Available In order to understand the dominant factors of the physical properties of ice in ice thermodynamics and mechanics, in-situ observations of ice growth and decay processes were carried out. Two samplings were conducted in the fast and steady ice growth stages. Ice pieces were used to observe ice crystals and gas bubbles in ice, and to measure the ice density. Vertical profiles of the type and size of ice crystals, shape and size of gas bubbles, and gas bubble content, as well as the ice density, were obtained. The results show that the upper layer of the ice pieces is granular ice and the lower layer is columnar ice; the average crystal size increases with the ice depth and remains steady in the fast and steady ice growth stages; the shape of gas bubbles in the upper layer of ice pieces is spherical with higher total content, and the shape in the middle and lower layers is cylinder with lower total content; the gas bubble size and content vary with the ice growth stage; and the ice density decreases with the increase of the gas bubble content.

  8. Lubricating and waxy esters, I. Synthesis, crystallization, and melt behavior of linear monoesters.

    Science.gov (United States)

    Bouzidi, Laziz; Li, Shaojun; Di Biase, Steve; Rizvi, Syed Q; Narine, Suresh S

    2012-01-01

    Four pure jojoba wax-like esters (JLEs), having carbon chain length of 36, 40 (two isomers) and 44, were prepared by Steglish esterification of fatty acids (or acid chlorides) with fatty alcohols at room temperature. Calorimetric and diffraction data was used to elucidate the phase behavior of the esters. The primary thermal parameters (crystallization and melting temperatures) obtained from the DSC of the symmetrical molecules correspond well with the carbon numbers of the JLEs. However, the data also suggests that carbon number is not the only factor since the symmetry of the molecule also plays a significant role in the phase behavior. Overall, the JLEs show very little polymorphic activity at the experimental conditions used, suggesting that they are likely to transform the same way during melting as well as crystallization, a characteristic which may be useful in designing new waxes and lubricants. The XRD data clearly show that the solid phase in all samples consists of a mixture of a β-phase and a β'-phase; fully distinguishable by their characteristic diffraction peaks. Subtle differences between the subcell patterns and phase development of the samples were observed. Different layering of the samples was also observed, understandably because of the chain length differences between the compounds. The long spacings were perfectly linearly proportional to the number of carbon atoms. The length of the ester layers with n carbon atoms can be calculated by a formula similar to that used for the layers in linear alkane molecules. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

  9. Crystallization of TiO2 Nanotubes by In Situ Heating TEM

    KAUST Repository

    Casu, Alberto

    2018-01-15

    The thermally-induced crystallization of anodically grown TiO2 amorphous nanotubes has been studied so far under ambient pressure conditions by techniques such as differential scanning calorimetry and in situ X-ray diffraction, then looking at the overall response of several thousands of nanotubes in a carpet arrangement. Here we report a study of this phenomenon based on an in situ transmission electron microscopy approach that uses a twofold strategy. First, a group of some tens of TiO2 amorphous nanotubes was heated looking at their electron diffraction pattern change versus temperature, in order to determine both the initial temperature of crystallization and the corresponding crystalline phases. Second, the experiment was repeated on groups of few nanotubes, imaging their structural evolution in the direct space by spherical aberration-corrected high resolution transmission electron microscopy. These studies showed that, differently from what happens under ambient pressure conditions, under the microscope’s high vacuum (p < 10−5 Pa) the crystallization of TiO2 amorphous nanotubes starts from local small seeds of rutile and brookite, which then grow up with the increasing temperature. Besides, the crystallization started at different temperatures, namely 450 and 380 °C, when the in situ heating was performed irradiating the sample with electron beam energy of 120 or 300 keV, respectively. This difference is due to atomic knock-on effects induced by the electron beam with diverse energy.

  10. Effect of sucrose polyesters on crystallization rate of vegetable ghee: solid fat content study

    Directory of Open Access Journals (Sweden)

    Ibrahim Nasir, Mohammad

    2003-12-01

    Full Text Available Crystallization rate of partial hydrogenated blend of soybean oil and cottonseed oil used for making vegetable ghee (vanaspati was investigated, by solid fat content (SFC using pulsed nuclear magnetic resonance (p-NMR. The effects of adding sucrose fatty acid esters or sucrose polyesters (SPE on the crystallization rate of the blend fat were studied. Sucrose tetrastearate DK ester F-10 (stearate 70% - palmitate 30% was added to the fat at different concentration, namely 0.5% and 1.0%. Blank sample and sample containing 0.5% and 1.0% DK ester F-10 / (DK F-10 were chosen to measure the change in SFC at constant temperature of 15ºC for a period of 25 hr. Five determinations of SFC were taken to the fat samples during the 25 hr i.e. 2,5,9,13 and 25th hr. SFC vs. time of crystallization of the three samples showed continuous increasing in SFC in all samples during the 25 hr, with sharp increasing at the first two hours. Samples containing 0.0% and 0.5% DK F-10, showed no significant difference in SFC during the first thirteen hours, while sample containing 1.0% DK F-10, showed higher SFC than the other two samples, through out the period. The amount of SFC for 1.0% DK F-10 sample at the 13th hour is equal to the SFC of the blank (0.0% sample at the 25th hour. Melting point of the same samples increased with the increasing DK F-10 concentration in the fat samples. The results of SFC make it sure that the addition of 1.0% DK F- 10 will shorten the time required for the crystallization of vegetable ghee while the addition of 0.5% will not have significant effect.Se ha investigado, mediante el contenido en grasa sólida (SFC por resonancia magnética nuclear pulsada (p-NMR, la velocidad de cristalización de mezcla de aceite de la soja y aceite de semilla del algodón parcialmente hidrogenada utilizada en la elaboración de ghee vegetal (vanaspati. Se han estudiado los efectos de añadir ésteres de sacarosa de ácidos grasos o poliésteres de

  11. Auto-oscillations of temperature and defect density in impure crystals under irradiation

    International Nuclear Information System (INIS)

    Selishchev, P.A.; Sugakov, V.I.

    1990-01-01

    Appearance of auto-oscillations in temperature and defect density of impurity crystals under irradiation is studied. It is shown that at certain critical parameters stationary distribution of temperature and defect density of the sample irradiated becomes unstable as regards the formation of temporal dissipative structures: auto-oscillations of temperature and defect density. Critical parameters are determined (the rate of defect formation, temperature of crystal environment, etc.) and the frequency of appearing auto-oscillations, its dependence on irradiation conditions and crystal properties are found

  12. The Crystal Hotel: A Microfluidic Approach to Biomimetic Crystallization.

    Science.gov (United States)

    Gong, Xiuqing; Wang, Yun-Wei; Ihli, Johannes; Kim, Yi-Yeoun; Li, Shunbo; Walshaw, Richard; Chen, Li; Meldrum, Fiona C

    2015-12-02

    A "crystal hotel" microfluidic device that allows crystal growth in confined volumes to be studied in situ is used to produce large calcite single crystals with predefined crystallographic orientation, microstructure, and shape by control of the detailed physical environment, flow, and surface chemistry. This general approach can be extended to form technologically important, nanopatterned single crystals. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Large-sized SmBCO single crystals with T sub c over 93 K grown in atmospheric ambient by crystal pulling

    CERN Document Server

    Yao Xin; Shiohara, Y

    2003-01-01

    Sm sub 1 sub + sub x Ba sub 2 sub - sub x Cu sub 3 O sub z (SmBCO) single crystals were grown under atmospheric ambient by the top-seeded solution growth method. Inductively coupled plasma results indicate that there is negligible Sm substitution for Ba sites in the grown SmBCO crystals, although they crystallized from different Ba-Cu-O solvents with a wide composition range (Ba/Cu ratio of 0.5-0.6). As a result, these crystals show high superconducting critical transition temperature values (T sub c) of over 93 K with a sharp transition width after oxygenation. A large-sized crystal with an a-b plane of 23 x 22 mm sup 2 and a c-axis of 19 mm was obtained at a high growth rate of nearly 0.13 mm h sup - sup 1. In short, with more controllable thermodynamic parameters, SmBCO single crystals can readily achieve both large size and high superconducting properties. (rapid communication)

  14. Carboxylic acids in crystallization of macromolecules: learning from successful crystallization experiments.

    Science.gov (United States)

    Offermann, Lesa R; He, John Z; Mank, Nicholas J; Booth, William T; Chruszcz, Maksymilian

    2014-03-01

    The production of macromolecular crystals suitable for structural analysis is one of the most important and limiting steps in the structure determination process. Often, preliminary crystallization trials are performed using hundreds of empirically selected conditions. Carboxylic acids and/or their salts are one of the most popular components of these empirically derived crystallization conditions. Our findings indicate that almost 40 % of entries deposited to the Protein Data Bank (PDB) reporting crystallization conditions contain at least one carboxylic acid. In order to analyze the role of carboxylic acids in macromolecular crystallization, a large-scale analysis of the successful crystallization experiments reported to the PDB was performed. The PDB is currently the largest source of crystallization data, however it is not easily searchable. These complications are due to a combination of a free text format, which is used to capture information on the crystallization experiments, and the inconsistent naming of chemicals used in crystallization experiments. Despite these difficulties, our approach allows for the extraction of over 47,000 crystallization conditions from the PDB. Initially, the selected conditions were investigated to determine which carboxylic acids or their salts are most often present in crystallization solutions. From this group, selected sets of crystallization conditions were analyzed in detail, assessing parameters such as concentration, pH, and precipitant used. Our findings will lead to the design of new crystallization screens focused around carboxylic acids.

  15. On dewetting of thin films due to crystallization (crystallization dewetting).

    Science.gov (United States)

    Habibi, Mehran; Rahimzadeh, Amin; Eslamian, Morteza

    2016-03-01

    Drying and crystallization of a thin liquid film of an ionic or a similar solution can cause dewetting in the resulting thin solid film. This paper aims at investigating this type of dewetting, herein termed "crystallization dewetting", using PbI2 dissolved in organic solvents as the model solution. PbI2 solid films are usually used in X-ray detection and lead halide perovskite solar cells. In this work, PbI2 films are fabricated using spin coating and the effect of major parameters influencing the crystallization dewetting, including the type of the solvent, solution concentration, drying temperature, spin speed, as well as imposed vibration on the substrate are studied on dewetting, surface profile and coverage, using confocal scanning laser microscopy. Simplified hydrodynamic governing equations of crystallization in thin films are presented and using a mathematical representation of the process, it is phenomenologically demonstrated that crystallization dewetting occurs due to the absorption and consumption of the solution surrounding a growing crystal. Among the results, it is found that a low spin speed (high thickness), a high solution concentration and a low drying temperature promote crystal growth, and therefore crystallization dewetting. It is also shown that imposed vibration on the substrate can affect the crystal size and crystallization dewetting.

  16. The Morse code effect: A crystal-crystal transformation observed in gel-grown lead (II) oxalate crystals

    Science.gov (United States)

    Lisgarten, J. N.; Marks, J. A.

    2018-05-01

    This paper reports on an unusual crystal-crystal transformation phenomenon, which we have called the Morse Code Effect, based on the change in appearance of lead(II) oxalate crystals grown in agarose gels.

  17. Fabrication and properties of gallium metallic photonic crystals

    International Nuclear Information System (INIS)

    Kozhevnikov, V.F.; Diwekar, M.; Kamaev, V.P.; Shi, J.; Vardeny, Z.V.

    2003-01-01

    Gallium metallic photonic crystals with 100% filling factor have been fabricated via infiltration of liquid gallium into opals of 300-nm silica spheres using a novel high pressure-high temperature technique. The electrical resistance of the Ga-opal crystals was measured at temperatures from 10 to 280 K. The data obtained show that Ga-opal crystals are metallic network with slightly smaller temperature coefficient of resistivity than that for bulk gallium. Optical reflectivity of bulk gallium, plain opal and several Ga-opal crystals were measured at photon energies from 0.3 to 6 eV. A pronounced photonic stop band in the visible spectral range was found in both the plain and Ga infiltrated opals. The reflectivity spectra also show increase in reflectivity below 0.6 eV; which we interpret as a significantly lower effective plasma frequency of the metallic mesh in the infiltrated opal compare to the plasma frequency in the pure metal

  18. LASER PROCESSING ON SINGLE CRYSTALS BY UV PULSE LASER

    OpenAIRE

    龍見, 雅美; 佐々木, 徹; 高山, 恭宜

    2009-01-01

    Laser processing by using UV pulsed laser was carried out on single crystal such as sapphire and diamond in order to understand the fundamental laser processing on single crystal. The absorption edges of diamond and sapphire are longer and shorter than the wave length of UV laser, respectively. The processed regions by laser with near threshold power of processing show quite different state in each crystal.

  19. Viscoelastic modes in chiral liquid crystals

    Indian Academy of Sciences (India)

    amit@fs.rri.local.net (Amit Kumar Agarwal)

    our studies on the viscoelastic modes of some chiral liquid crystals using dynamic light scattering. We discuss viscoelastic ... In the vicinity of the direct beam for a sample aligned in the Bragg mode and. 297 ... experimental investigations on these modes. Duke and Du ..... scattering volume is not true in practice. In an actual ...

  20. Nonlinear spin wave coupling in adjacent magnonic crystals

    Energy Technology Data Exchange (ETDEWEB)

    Sadovnikov, A. V., E-mail: sadovnikovav@gmail.com; Nikitov, S. A. [Laboratory “Metamaterials,” Saratov State University, Saratov 410012 (Russian Federation); Kotel' nikov Institute of Radioengineering and Electronics, Russian Academy of Sciences, Moscow 125009 (Russian Federation); Beginin, E. N.; Morozova, M. A.; Sharaevskii, Yu. P.; Grishin, S. V.; Sheshukova, S. E. [Laboratory “Metamaterials,” Saratov State University, Saratov 410012 (Russian Federation)

    2016-07-25

    We have experimentally studied the coupling of spin waves in the adjacent magnonic crystals. Space- and time-resolved Brillouin light-scattering spectroscopy is used to demonstrate the frequency and intensity dependent spin-wave energy exchange between the side-coupled magnonic crystals. The experiments and the numerical simulation of spin wave propagation in the coupled periodic structures show that the nonlinear phase shift of spin wave in the adjacent magnonic crystals leads to the nonlinear switching regime at the frequencies near the forbidden magnonic gap. The proposed side-coupled magnonic crystals represent a significant advance towards the all-magnonic signal processing in the integrated magnonic circuits.