Solid-state properties and crystallization behavior of PHA-739521 polymorphs.

PubMed

Sun, Changquan Calvin

2006-08-17

PHA-739521 is an experimental compound that exhibits polymorphism. The two anhydrous crystal forms, I and II, are characterized using powder X-ray diffractometry, thermal analyses, moisture sorption gravimetry. Both Forms I and II are non-hygroscopic and are stable to compaction pressure. The melting temperature is about 152 degrees C for Form I and 168 degrees C for Form II. Forms I and II are enantiotropically related where Form I is more stable below a transition temperature of approximately 70 degrees C. Crystallization behavior of this compound from solutions and during heating is also studied. Information obtained is used to design an appropriate crystallization process to successfully manufacture desired polymorph at large scale.

Study of multilayered SiGe semiconductor structures by X-ray diffractometry, grazing-incidence X-ray reflectometry, and secondary-ion mass spectrometry

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

Yunin, P. A., E-mail: yunin@ipmras.ru; Drozdov, Yu. N.; Drozdov, M. N.

2013-12-15

In this publication, we report the results of studying a multilayerd nonperiodic SiGe/Si structure by the methods of X-ray diffractometry, grazing-angle X-ray reflectometry, and secondary-ion mass spectrometry (SIMS). Special attention is paid to the processing of the component distribution profile using the SIMS method and to consideration of the most significant experimental distortions introduced by this method. A method for processing the measured composition distribution profile with subsequent consideration of the influence of matrix effects, variation in the etching rate, and remnants of ion sputtering is suggested. The results of such processing are compared with a structure model obtained uponmore » combined analysis of X-ray diffractometry and grazing-angle reflectometry data. Good agreement between the results is established. It is shown that the combined use of independent techniques makes it possible to improve the methods of secondary-ion mass spectrometry and grazing-incidence reflectometry as applied to an analysis of multilayered heteroepitaxial structures (to increase the accuracy and informativity of these methods)« less

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

DOE PAGES

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

2015-04-06

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

Structural properties of H-implanted InP crystals

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

Bocchi, C.; Franzosi, P.; Lazzarini, L.

1993-07-01

H has been implanted in InP crystals at the energy E [equals] 100 keV and at different doses ranging from [sigma] [equals] 1 x 10[sup 13] to [sigma] [equals] 5 x 10[sup 16] cm[sup [minus]2]. The depth dependence of the elastic lattice strain has been investigated by high resolution X-ray diffractometry. The implantation produces a lattice dilation. The strain increases with increasing depth, reaches the maximum at about 0.75 [mu]m, and then decreases rapidly; moreover the maximum strain is proportional to the dose. No extended crystal defects have been detected by transmission electron microscopy up to [sigma] <1 x 10[supmore » 16] cm[sup [minus]2] a buried amorphous layer 28 nm in thickness has been observed at the same depth where the strain is maximum. The thickness of the amorphous layer increases by further increasing the dose and reaches a value of about 0.18 [mu]m for [sigma] [equals] 5 x 10[sup 16] cm[sup [minus]2].« less

Molecular beam epitaxial growth and structural characterization of ZnS on (001) GaAs

NASA Technical Reports Server (NTRS)

Benz, R. G., II; Huang, P. C.; Stock, S. R.; Summers, C. J.

1988-01-01

The effect of surface nucleation processes on the quality of ZnS layers grown on (001) GaAs substrates by molecular beam epitaxy is reported. Reflection high energy electron diffraction indicated that nucleation at high temperatures produced more planar surfaces than nucleation at low temperatures, but the crystalline quality as assessed by X-ray double crystal diffractometry is relatively independent of nucleation temperature. A critical factor in layer quality was the initial roughness of the GaAs surfaces.

Application of film-casting technique to investigate drug-polymer miscibility in solid dispersion and hot-melt extrudate.

PubMed

Parikh, Tapan; Gupta, Simerdeep Singh; Meena, Anuprabha K; Vitez, Imre; Mahajan, Nidhi; Serajuddin, Abu T M

2015-07-01

Determination of drug-polymer miscibility is critical for successful development of solid dispersions. This report details a practical method to predict miscibility and physical stability of drug with various polymers in solid dispersion and, especially, in melt extrudates by applying a film-casting technique. Mixtures of itraconazole (ITZ) with hydroxypropylmethylcellulose phthalate (HPMCP), Kollidon(®) VA 64, Eudragit(®) E PO, and Soluplus(®) were film-casted, exposed to 40°C/75% RH for 1 month and then analyzed using differential scanning calorimetry (DSC), powder X-ray diffractometry, and polarized light microscopy (PLM). ITZ had the highest miscibility with HPMCP, being miscible at drug to polymer ratio of 6:4 (w/w). There was a downward trend of lower miscibility with Soluplus(®) (miscible at 3:7, w/w, and a few microcrystals present at 4:6, w/w), Kollidon(®) VA 64 (2:8, w/w) and Eudragit(®) E PO (<1:9, w/w). PLM was found more sensitive to detect drug crystallization than DSC and powder X-ray diffractometry. There was general correlation between results of film casting and hot-melt extrusion (HME) using a twin screw extruder. For ITZ-Soluplus(®) mixtures, HME at 4:6 (w/w) resulted in a single phase, whereas drug crystallization was observed at higher drug load. HME of ITZ-Kollidon(®) VA 64 mixtures also correlated well with the miscibility predicted by film casting. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Formulation and Solid State Characterization of Nicotinamide-based Co-crystals of Fenofibrate

PubMed Central

Shewale, Sheetal; Shete, A. S.; Doijad, R. C.; Kadam, S. S.; Patil, V. A.; Yadav, A. V.

2015-01-01

The present investigation deals with formulation of nicotinamide-based co-crystals of fenofibrate by different methods and solid-state characterization of the prepared co-crystals. Fenofibrate and nicotinamide as a coformer in 1:1 molar ratio were used to formulate molecular complexes by kneading, solution crystallization, antisolvent addition and solvent drop grinding methods. The prepared molecular complexes were characterized by powder X-ray diffractometry, differential scanning calorimetry, Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy and in vitro dissolution study. Considerable improvement in the dissolution rate of fenofibrate from optimized co-crystal formulation was due to an increased solubility that is attributed to the super saturation from the fine co-crystals is faster because of large specific surface area of small particles and prevention of phase transformation to pure fenofibrate. In vitro dissolution study showed that the formation of co-crystals improves the dissolution rate of fenofibrate. Nicotinamide forms the co-crystals with fenofibrate, theoretically and practically. PMID:26180279

X-Ray Diffraction of Intermetallic Compounds: A Physical Chemistry Laboratory Experiment

ERIC Educational Resources Information Center

Varberg, Thomas D.; Skakuj, Kacper

2015-01-01

Here we describe an experiment for the undergraduate physical chemistry laboratory in which students synthesize the intermetallic compounds AlNi and AlNi3 and study them by X-ray diffractometry. The compounds are synthesized in a simple one-step reaction occurring in the solid state. Powder X-ray diffractograms are recorded for the two compounds…

Ultrastructure of selected struvite-containing urinary calculi from cats.

PubMed

Neumann, R D; Ruby, A L; Ling, G V; Schiffman, P S; Johnson, D L

1996-01-01

To elucidate the ultrastructural details of struvite-containing urinary calculi from cats. Specimens studied were inclusive of the range of textures visible during preliminary analysis by use of a stereoscopic dissecting microscope. Textural types, which were used to infer crystal growth conditions, were differentiated with regard to crystal habit, crystal size, growth orientation, and primary porosity. Thirty specimens were selected from a collection of approximately 1,600 feline urinary calculi: 20 of these were composed entirely of struvite, and 10 consisted of struvite and calcium phosphate (apatite). Qualitative and quantitative analyses of specimens included use of plain and polarized light microscopy, x-ray diffractometry, scanning electron microscopy with backscattered electron imagery, x-ray fluorescence scans, and electron probe microanalysis. Four textural types were recognized among struvite calculi, whereas 2 textural types of struvite-apatite calculi were described. The presence of minute, well interconnected primary pores in struvite-containing urinary calculi from cats is an important feature, which may promote possible interaction of calculi with changes in urine composition. Primary porosity, which can facilitate interaction between the calculus and changing urine composition, may explain the efficacy of dietary or medicinal manipulations to promote the dissolution of struvite-containing uroliths from this species.

Ion-induced crystal damage during plasma-assisted MBE growth of GaN layers

NASA Astrophysics Data System (ADS)

Kirchner, V.; Heinke, H.; Birkle, U.; Einfeldt, S.; Hommel, D.; Selke, H.; Ryder, P. L.

1998-12-01

Gallium nitride layers were grown by plasma-assisted molecular-beam epitaxy on (0001)-oriented sapphire substrates using an electron cyclotron resonance (ECR) and a radio frequency (rf) plasma source. An applied substrate bias was varied from -200 to +250 V, resulting in a change of the density and energy of nitrogen ions impinging the growth surface. The layers were investigated by high-resolution x-ray diffractometry and high-resolution transmission electron microscopy (HRTEM). Applying a negative bias during growth has a marked detrimental effect on the crystal perfection of the layers grown with an ECR plasma source. This is indicated by a change in shape and width of (0002) and (202¯5) reciprocal lattice points as monitored by triple axis x-ray measurements. In HRTEM images, isolated basal plane stacking faults were found, which probably result from precipitation of interstitial atoms. The crystal damage in layers grown with a highly negative substrate bias is comparable to that observed for ion implantation processes at orders of magnitude larger ion energies. This is attributed to the impact of ions on the growing surface. None of the described phenomena was observed for the samples grown with the rf plasma source.

Synthesis of vaterite and aragonite crystals using biomolecules of tomato and capsicum

NASA Astrophysics Data System (ADS)

Chen, Long; Xu, Wang-Hua; Zhao, Ying-Guo; Kang, Yan; Liu, Shao-Hua; Zhang, Zai-Yong

2012-12-01

In this paper, biomimetic synthesis of calcium carbonate (CaCO3) in the presence of biomolecules of two vegetables-tomato and capsicum is investigated. Scanning electron microscopy and X-ray powder diffractometry were used to characterize the CaCO3 obtained. The biomolecules in the extracts of two vegetables are determined by UV-vis or FTIR. The results indicate that a mixture of calcite and vaterite spheres constructed from small particles is produced with the extract of tomato, while aragonite rods or ellipsoids are formed in the presence of extract of capsicum. The possible formation mechanism of the CaCO3 crystals with tomato biomolecules can be interpreted by particle-aggregation based non-classical crystallization laws. The proteins and/or other biomolecules in tomato and capsicum may control the formation of vaterite and aragonite crystals by adsorbing onto facets of them.

Solid state of CG-400549, a novel FabI inhibitor: characterization, dissolution, transformation.

PubMed

Kim, Bo-Yeon; Sohn, Young-Taek

2011-05-01

The polymorphic and pseudopolymorphic forms of CG-400549, a novel FabI inhibitor with potent in vivo activity were prepared and characterized by differential scanning calorimetry (DSC), powder X-ray diffractometry (PXRD) and thermogravimetric analysis (TG). Seven crystal forms of CG-400549, one anhydrate and six solvates, have been isolated by recrystallization and the DSC and PXRD patterns of the seven crystal forms of CG-400549 were different respectively. The dissolution patterns of these seven crystal forms of CG-400549 were studied and they showed significant differences in the dissolution rate. After storage of 1 month at 0% RH (silica gel, 20°C), 52% RH (saturated solution of Na(2)Cr(2)O(7)2H(2)O/20°C) and 95% RH (saturated solution of Na(2)HPO(4)/20°C), all crystal forms were not transformed.

Self-propagating high-temperature synthesis and luminescent properties of ytterbium doped rare earth (Y, Sc, Lu) oxides nanopowders

NASA Astrophysics Data System (ADS)

Permin, D. A.; Novikova, A. V.; Balabanov, S. S.; Gavrishchuk, E. M.; Kurashkin, S. V.; Savikin, A. P.

2018-04-01

This paper describes a comparative study of structural and luminescent properties of 5%Yb-doped yttrium, scandium, and lutetium oxides (Yb:RE2O3) powders and ceramics fabricated by self-propagating high-temperature synthesis. According to X-ray diffractometry and electron microscopy the chosen method ensures preparation of low-agglomerated cubic Ctype crystal structured powders at one step. No crucial differences in luminescence spectra were found the Yb:RE2O3 powders and ceramics. It was shown that the emission lifetimes of the Yb:RE2O3 powders are lowered by crystal structure defects, while its values for ceramics samples are compared to that of monocrystals and more influenced by rare earth impurities.

5-Arylidene derivatives of Meldrum's acid: Synthesis, structural characterization using single crystal and powder crystal X-ray diffraction, and electronic properties

NASA Astrophysics Data System (ADS)

Dey, Tanusri; Ghosh, Soumen; Ghosh, Somnath; Mukherjee, Alok Kumar

2015-07-01

Four 5-arylidene derivatives of Meldrum's acid, 5-(4-chlorobenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (2), 5-(3-hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (3), 5-(3,4-dimethoxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (4) and 5-(2,4-dimethoxy benzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (5) have been synthesized and their crystal structures have been determined using single crystal X-ray diffractometry for 2, 4 and 5 and X-ray powder diffraction for 3. The nature of intermolecular interactions in 2-5 has been analyzed through Hirshfeld surfaces and 2D fingerprint plots. The DFT optimized molecular geometries in 2-5 agree closely with those obtained from the crystallographic studies. The crystal packing in 2-5 exhibits an interplay of Osbnd H⋯O, Csbnd H⋯O, Csbnd H⋯Cl and Csbnd H⋯π (arene) hydrogen bonds and π⋯π interactions, which assemble molecules into three-dimensional architecture in 2, 3 and 5 and two-dimensional framework in 4. The Hirshfeld surface analyses of 2-5, Meldrum's acid (1) and a few related 5-arylidene derivatives of Meldrum's acid retrieved from the Cambridge Structural Database (CSD) indicate that about 85% of the Hirshfeld surface area (72% in 2 where H⋯Cl contribution is about 13%) in this class of compounds are due to H⋯H, O⋯H and C⋯H contacts. The HOMO-LUMO energy gap (>2.2 eV) in 2-5 indicates a significant degree of internal charge transfer within the molecule.

An x-ray diffraction study of microstructural deformation induced by cyclic loading of selected steel

NASA Astrophysics Data System (ADS)

Fourspring, Patrick Michael

X-ray double crystal diffractometry (XRDCD) and X-ray scanning diffractometry (XRSD) were used to assess cyclic microstructural deformation in a face centered cubic (fcc) steel (AISI304) and a body centered cubic (bcc) steel (SA508 class 2). The objectives of the investigation were to determine if X-ray diffraction could be used effectively to monitor cyclic microstructural deformation in polycrystalline Fe alloys and to study the distribution of the microstructural deformation induced by cyclic loading in these alloys. The approach used in the investigation was to induce fatigue damage in a material and to characterize the resulting microstructural deformation at discrete fractions of the fatigue life of the material. Also, characterization of microstructural deformation was carried out to identify differences in the accumulation of damage from the surface to the bulk, focusing on the following three regions: near surface (0-10 mum), subsurface (10-300 mum), and bulk. Characterization of the subsurface region was performed only on the AISI304 material because of the limited availability of the SA508 material. The results from the XRDCD data indicate a measurable change induced by fatigue from the initial state to subsequent states of both the AISI304 and the SA508 materials. The results from the XRSD data show similar but less coherent trends than the results from the XRDCD data. Therefore, the XRDCD technique was shown to be sensitive to the microstructural deformation caused by fatigue in steels; thus, the technique can be used to monitor fatigue damage in steels. In addition, for the AISI304 material, the level of cyclic microstructural deformation in the bulk material was found to be greater than the level in the near surface material. In contrast, previous investigations have shown that the deformation is greater in the near surface than the bulk for Al alloys and bcc Fe alloys.

Impact of plant matrix polysaccharides on cellulose produced by surface-tethered cellulose synthases.

PubMed

Basu, Snehasish; Omadjela, Okako; Zimmer, Jochen; Catchmark, Jeffrey M

2017-04-15

Surface immobilized BcsA-B cellulose synthases synthesize crystalline cellulose II under in vitro conditions and were used to explore the interaction between cellulose and hemicelluloses and pectin. The morphology of the cellulose microfibrils changed in the presence of xyloglucan and glucomannan, while pectin did not significantly impact morphology. X-ray diffractometry and FT-IR spectroscopy indicated that crystal size and crystallinity were significantly affected by xyloglucan and glucomannan but not altered by pectin. Glucomannan had the most significant impact on the structure of cellulose and inhibits crystallization. The presence of xyloglucan and glucomannan prevents the proper assembly of cellulose microfibrils and changes the crystalline properties of cellulose II in in vitro conditions, but did not have any impact on cellulose allomorph. Copyright © 2017 Elsevier Ltd. All rights reserved.

Investigation of recrystallization of amorphous trehalose through hot-humidity stage X-ray powder diffraction.

PubMed

Jójárt-Laczkovich, Orsolya; Katona, Gábor; Aigner, Zoltán; Szabó-Révész, Piroska

2016-12-01

The aim of this work was an investigation of the physical changes of the amorphous model material spray-dried trehalose through the use of various analytical techniques and to identify a suitable, rapid method able to quantify the changes. The crystallinity changes and recrystallization process of amorphous samples were investigated by hot-humidity stage X-ray powder diffractometry (HH-XRPD) with fresh samples, conventional X-ray powder diffractometry (XRPD) used stored samples and by differential scanning calorimetry (DSC). The data from the three methods were compared and the various forms of trehalose were analysed. HH-XRPD demonstrated that the recrystallization began at 40 and 60°C up to 45% RH and at 70°C up to 30% RH into dihydrate form. At 70°C up to 60% RH the anhydrous form of trehalose appeared too. Conventional XRPD results showed, that in the 28days stored samples the dihydrate form was detected at 40°C, 50% RH. Storage at 60°C, 40% RH resulted in the appearance of the anhydrous form and at 60°C, 50% RH both polymorphic forms were detected. By carrying out the DSC measurements at different temperatures the fraction of recrystallized trehalose dihydrate was detected. The recrystallization investigated by HH-XRPD and DSC followed Avrami kinetics, the calculated rate constants of isothermal crystallization (K) were same. Both HH-XRPD and conventional XRPD was suitable for the detection of the physical changes of the amorphous model material. DSC measurements showed similar results as HH-XRPD. Primarily HH-XRPD could be suggested for prediction, because the method is fast and every changes could be studied on one sample. Copyright © 2016 Elsevier B.V. All rights reserved.

The polymorphic and mesomorphic behavior of four esters of cholesterol.

NASA Technical Reports Server (NTRS)

Merritt, W. G.; Cole, G. D.; Walker, W. W.

1971-01-01

The techniques of differential scanning calorimetry, X-ray powder diffractometry, and positron annihilation have been used to study the polymorphic and mesomorphic behavior of the following esters of cholesterol: cholesteryl formate, cholesteryl butyrate, cholesteryl benzoate, and cholesteryl cinnamate. Each of these compounds exhibits a single mesophase of the cholesteric type. The solid phase formed from the melt for each ester was observed to be structurally different from the solid phase obtained from solution. Solvents from which the solution-grown samples were crystallized were as follows: cholesteryl formate and cholesteryl butyrate from acetone, cholesteryl benzoate from benzene, and cholesteryl cinnamate from 2-butanone.

Polymorphic polytypic transition induced in crystals by interaction of spirals and 2D growth mechanisms

NASA Astrophysics Data System (ADS)

Aquilano, Dino; Veesler, Stéphane; Astier, Jean Pierre; Pastero, Linda

2003-01-01

The relationship between crystal polymorphism and polytypism can be revealed by surface patterns through the interlacing of the growth spirals. Simple high-symmetry structures as SiC, ZnS, CdI2 and more complex low-symmetry layered structures as n-paraffins, n-alcohols and micas are concerned with polymorphic-polytypic transition. In this paper, we will show for the first time, through in situ AFM observations and X-ray diffractometry, that a protein polymorph (P2 12 12 1α-amylase) locally changes, during growth, to a monoclinic P2 1 polytype, thanks to the screw dislocation activity. The interplay between spiral steps and 2D nuclei of the polytypes coexisting in the same crystalline individual allows to foresee the consequences on the crystal quality. The discussion is extended to other mineral and biological molecules and a new general rule is proposed to explain the interactions between surface patterns and the bulk crystal structure.

Modification of the crystal habit of celecoxib for improved processability.

PubMed

Banga, Sheere; Chawla, Garima; Varandani, Deepak; Mehta, B R; Bansal, Arvind K

2007-01-01

Crystallization is often used in the pharmaceutical industry for purification and isolation of drugs, and also as a means of generating polymorphs or isomorphs. The aim of this study was to investigate the role of extrinsic crystallization parameters on the crystallized product, with special emphasis on improving the mechanical properties of acicular celecoxib. Celecoxib isomorphs were prepared using different techniques (solvent crystallization and vapour diffusion) and crystallization conditions (solvents, stirring, degree of supersaturation, crystallization temperature and seeding). Powder X-ray diffractometry, spectroscopic and thermal methods were used to investigate physical characteristics of crystals. Growth kinetics and aggregation dynamics of crystallization in polar and non-polar solvents were simulated using a dynamic light scattering method. The quick appearance of broad peaks over the range of 10-8000 nm in chloroform during crystallization simulation studies indicated faster aggregation in non-polar solvents. Aspect ratio, flow, compressibility and surface area of recrystallized products were also determined. Surface topography was determined by atomic force microscopy and the lath-shaped crystals (aspect ratio of 2-4) exhibited a roughness index of 1.79 in comparison with 2.92 for needles. Overall, the lath-shaped isomorphs exhibited improved flow and better compressibility.

X-ray structural studies and physicochemical characterization of (E)-6-(3,4-dimethoxyphenyl)-1-ethyl-4-mesitylimino-3-methyl- 3,4-dihydro-2(1H)-pyrimidinone polymorphs.

PubMed

Miyamae, A; Kitamura, S; Tada, T; Koda, S; Yasuda, T

1991-10-01

The polymorphism of (E)-6-(3,4-dimethoxyphenyl)-1-ethyl-4-mesitylimino-3-methyl-3,4-di hydro- 2(1 H)-pyrimidinone (FK664; 1) was characterized by using X-ray powder diffractometry, differential scanning calorimetry (DSC), and IR spectroscopy. Structures of two polymorphs (Forms A and B) were determined by X-ray crystallographic analysis. Form A crystallized in the monoclinic space group P2(1)/c, with a = 13.504(2), b = 6.733(1), c = 24.910(8) A, beta = 96.55(4) degrees, z = 4, and dcal = 1.203 g/cm3, while Form B crystallized in the same space group, with a = 8.067(2), b = 15.128(4), c = 18.657(4) A, beta = 102.34(3) degrees, z = 4, and dcal = 1.216 g/cm3. The conformational features of 1 were very similar between the two polymorphs. Compound 1, in both crystal forms, took an energetically reasonable conformation in three rigid planes, such as 2-pyrimidone, trimethylphenyl, and dimethoxyphenyl rings, but the molecules were packed in different ways between the two polymorphs. In the Form B crystal, a short contact was possible, to form pi-pi interactions between two dimethoxyphenyl groups related with the inversion center in the crystal lattice; this interaction seems to contribute to stabilizing the crystal structure of Form B. Both Forms A and B showed only one endothermic peak due to fusion at 115 and 140 degrees C, respectively, on the DSC thermograms; therefore, it is suggested that there are no transition points between the two polymorphs. The heats of fusion obtained from the DSC thermograms were 33.2(2) kJ/mol for Form A and 36.8(1) kJ/mol for Form B.(ABSTRACT TRUNCATED AT 250 WORDS)

Second amorphous-to-crystalline phase transformation in Cu(60)Ti(20)Zr(20) bulk metallic glass.

PubMed

Cao, Q P; Li, J F; Zhang, P N; Horsewell, A; Jiang, J Z; Zhou, Y H

2007-06-20

The second amorphous-to-crystalline phase transformation in Cu(60)Ti(20)Zr(20) bulk metallic glass was investigated by differential scanning calorimetry and x-ray diffractometry. The difference of the Gibbs free energies between the amorphous phase and the crystalline products during the transformation is estimated to be about 2.46 kJ mol(-1) at 753 K, much smaller than the 61 kJ mol(-1) obtained assuming that it is a polymorphic transformation. It was revealed that the phase transformation occurs through a eutectic crystallization of Cu(51)Zr(14) and Cu(2)TiZr, having an effective activation energy of the order of 400 kJ mol(-1). The average Avrami exponent n is about 2.0, indicating that the crystallization is diffusion controlled.

Solid state polymerization and crystallography of polyimide precursors. Ph.D. Thesis - Va. Univ.

NASA Technical Reports Server (NTRS)

Wakelyn, N. T.

1974-01-01

Although the production of crystallinity in a polymeric system has historically led to commerically useful properties, the polyimides, prized for their high temperature characteristics, as customarily synthesized by melt or solution casting, are amorphous. It is shown that polymide containing residual crystallinity can be synthesized by isothermal annealing of crystals of the salt of the diisopropyl ester of pyromellitic acid and phenylene diamine. The reaction is topochemical in that the geometry of the polymer product is dependent upon that of the crystalline precursor. Infrared spectroscopy reveals the presence of imide absorption in the polymer, while powder diffractometry suggests residual crystallinity. Single crystal X-ray analysis of the monomer yields a structure of chains of alternating acid and base suggesting that the monomer is amenable to polymerization with a minimum of geometrical disruption.

Quantitative measurement of indomethacin crystallinity in indomethacin-silica gel binary system using differential scanning calorimetry and X-ray powder diffractometry.

PubMed

Pan, Xiaohong; Julian, Thomas; Augsburger, Larry

2006-02-10

Differential scanning calorimetry (DSC) and X-ray powder diffractometry (XRPD) methods were developed for the quantitative analysis of the crystallinity of indomethacin (IMC) in IMC and silica gel (SG) binary system. The DSC calibration curve exhibited better linearity than that of XRPD. No phase transformation occurred in the IMC-SG mixtures during DSC measurement. The major sources of error in DSC measurements were inhomogeneous mixing and sampling. Analyzing the amount of IMC in the mixtures using high-performance liquid chromatography (HPLC) could reduce the sampling error. DSC demonstrated greater sensitivity and had less variation in measurement than XRPD in quantifying crystalline IMC in the IMC-SG binary system.

Preparation and Thermoelectric Properties of IR(sub x)Co(sub 1-x)Sb(sub 2) Alloys

NASA Technical Reports Server (NTRS)

Caillat, Thierry

1995-01-01

The preparation and characterization of the binary arsenopyrite compounds CoSb2 and IrSb2 and IrxCo1-xSb2 alloys is reported. Single crystals of CoSb2 were grown by the vertical gradient freeze technique from solution rich in antimony. Polycrystalline samples of IrSb2 and IrxCo1-xSb2 alloys were prepared by hot-pressing of prereacted elemental powders. Samples were investigated by X-ray diffractometry, microprobe analysis and density measurements. It was found that a range of solid solution exist in the system IrxCo1-xSb2 for 0.1

Sample holder for X-ray diffractometry

DOEpatents

Hesch, Victor L.

1992-01-01

A sample holder for use with X-ray diffractometers with the capability to rotate the sample, as well as to adjust the position of the sample in the x, y, and z directions. Adjustment in the x direction is accomplished through loosening set screws, moving a platform, and retightening the set screws. Motion translators are used for adjustment in the y and z directions. An electric motor rotates the sample, and receives power from the diffractometer.

Relationship between crystal structure and solid-state properties of pharmaceuticals

NASA Astrophysics Data System (ADS)

Sheth, Agam R.

This thesis strives to understand the structure-property relationships of some pharmaceutical crystals at the molecular level with emphasis on the effect of secondary processing on the solid phase. Using single crystal X-ray diffractometry (SCXRD), the structure of warfarin sodium 2-propanol adduct (W) was established to be a true solvate, contrary to previous reports. Using dynamic water vapor sorption, optical and environmental scanning electron microscopy, SCXRD, powder X-ray diffractometry (PXRD), volume computations and molecular modeling, the effect of relative humidity and temperature on the crystal structure of W was investigated. Ab initio calculations on piroxicam showed that the difference in energy between the two polymorphs, I and II, arises predominantly from the difference between their lattice energies. The detailed hydrogen bonding networks of the two polymorphs are described and compared using graph sets. Despite stabilization of the polymorphs by hydrogen bonds, pair-wise distribution function transforms show a loss of polymorphic memory upon cryogrinding the two polymorphs, leading to a difference in recrystallization behavior between amorphous piroxicam prepared from polymorphs I and II. Structural and solid-state changes of piroxicam polymorphs under mechanical stress were investigated using cryogenic grinding, PXRD, diffuse-reflectance solid-state ultraviolet-visible spectroscopy, 13C solid-state nuclear magnetic resonance spectroscopy, and diffuse-reflectance solid-state Fourier-transform infrared spectroscopy. Intermolecular proton transfer was found to accompany changes in phase and color observed upon cryogrinding the two polymorphs. Model-free and model-fitting studies of the dehydration kinetics of piroxicam monohydrate (PM) showed the dependence of activation energy ( Ea) on both isothermal and non-isothermal heating conditions, and on the fraction of conversion. In the constant-E a region, isothermal dehydration follows the two-dimensional phase boundary model, while non-isothermal dehydration follows a mechanism intermediate between two- and three-dimensional diffusion that cannot be described by any of the common models. Structural studies suggest that the complex hydrogen bond pattern in PM is responsible for the observed dehydration behavior. Ab initio calculations provide an explanation for the changes in the molecular and crystal structures accompanying the reversible change in hydration state between anhydrous piroxicam Form I and PM. The thesis further demonstrates the utility of model-free analysis in describing complex dehydration kinetics.

Mesoporous silica templated zirconia nanoparticles

NASA Astrophysics Data System (ADS)

Ballem, Mohamed A.; Córdoba, José M.; Odén, Magnus

2011-07-01

Nanoparticles of zirconium oxide (ZrO2) were synthesized by infiltration of a zirconia precursor (ZrOCl2·8H2O) into a SBA-15 mesoporous silica mold using a wet-impregnation technique. X-ray diffractometry and high-resolution transmission electron microscopy show formation of stable ZrO2 nanoparticles inside the silica pores after a thermal treatment at 550 °C. Subsequent leaching out of the silica template by NaOH resulted in well-dispersed ZrO2 nanoparticles with an average diameter of 4 nm. The formed single crystal nanoparticles are faceted with 110 surfaces termination suggesting it to be the preferred growth orientation. A growth model of these nanoparticles is also suggested.

CuLi2Sn and Cu2LiSn: Characterization by single crystal XRD and structural discussion towards new anode materials for Li-ion batteries.

PubMed

Fürtauer, Siegfried; Effenberger, Herta S; Flandorfer, Hans

2014-12-01

The stannides CuLi 2 Sn (CSD-427095) and Cu 2 LiSn (CSD-427096) were synthesized by induction melting of the pure elements and annealing at 400 °C. The phases were reinvestigated by X-ray powder and single-crystal X-ray diffractometry. Within both crystal structures the ordered CuSn and Cu 2 Sn lattices form channels which host Cu and Li atoms at partly mixed occupied positions exhibiting extensive vacancies. For CuLi 2 Sn, the space group F-43m. was verified (structure type CuHg 2 Ti; a =6.295(2) Å; wR 2 ( F ²)=0.0355 for 78 unique reflections). The 4( c ) and 4( d ) positions are occupied by Cu atoms and Cu+Li atoms, respectively. For Cu 2 LiSn, the space group P 6 3 / mmc was confirmed (structure type InPt 2 Gd; a =4.3022(15) Å, c =7.618(3) Å; wR 2 ( F ²)=0.060 for 199 unique reflections). The Cu and Li atoms exhibit extensive disorder; they are distributed over the partly occupied positions 2( a ), 2( b ) and 4( e ). Both phases seem to be interesting in terms of application of Cu-Sn alloys as anode materials for Li-ion batteries.

Synthesis of barium and strontium carbonate crystals with unusual morphologies using an organic additive

NASA Astrophysics Data System (ADS)

Chen, Long; Jiang, Jizhong; Bao, Zuben; Pan, Jian; Xu, Weibing; Zhou, Lili; Wu, Zhigang; Chen, Xu

2013-12-01

In this paper, strontium carbonate (SrCO3) and barium carbonate (BaCO3) crystals were synthesized in the presence of an organic additive-hexamethylenetetramine (HMT) using two CO2 sources. Scanning electron microscopy and X-ray powder diffractometry were used to characterize the products. The results showed that the morphologies of orthorhombic strontianite SrCO3 transformed from branch-like to flower-like, and to capsicum-like at last, while the morphologies of BaCO3 change from fiber-like to branchlike, and to rod-like finally with an increase of the molar ratio HMT/Sr2+ and HMT/Ba2+ from 0.2 to 10 using ammonium carbonate as CO2 source. When using diethyl carbonate instead of ammonium carbonate as CO2 source, SrCO3 flowers aggregated by rods and BaCO3 shuttles were formed. The possible formation mechanisms of SrCO3 and BaCO3 crystals obtained in different conditions were also discussed.

Reversible Li storage for nanosize cation/anion-disordered rocksalt-type oxyfluorides: LiMoO2 - x LiF (0 ≤ x ≤ 2) binary system

NASA Astrophysics Data System (ADS)

Takeda, Nanami; Hoshino, Satoshi; Xie, Lixin; Chen, Shuo; Ikeuchi, Issei; Natsui, Ryuichi; Nakura, Kensuke; Yabuuchi, Naoaki

2017-11-01

A binary system of LiMoO2 - x LiF (0 ≤ x ≤ 2), Li1+xMoO2Fx, is systematically studied as potential positive electrode materials for rechargeable Li batteries. Single phase and nanosized samples on this binary system are successfully prepared by using a mechanical milling route. Crystal structures and Li storage properties on the binary system are also examined. Li2MoO2F (x = 1), which is classified as a cation-/anion-disordered rocksalt-type structure and is a thermodynamically metastable phase, delivers a large reversible capacity of over 300 mAh g-1 in Li cells with good reversibility. Highly reversible Li storage is realized for Li2MoO2F consisting of nanosized particles based on Mo3+/Mo5+ two-electron redox as evidenced by ex-situ X-ray absorption spectroscopy coupled with ex-situ X-ray diffractometry. Moreover, the presence of the most electronegative element in the framework structure effectively increases the electrode potential of Mo redox through an inductive effect. From these results, potential of nanosized lithium molybdenum oxyfluorides for high-capacity positive electrode materials of rechargeable Li batteries are discussed.

Ultrasonication as a potential tool to predict solute crystallization in freeze-concentrates.

PubMed

Ragoonanan, Vishard; Suryanarayanan, Raj

2014-06-01

We hypothesize that ultrasonication can accelerate solute crystallization in freeze-concentrates. Our objective is to demonstrate ultrasonication as a potential predictive tool for evaluating physical stability of excipients in frozen solutions. The crystallization tendencies of lyoprotectants (trehalose, sucrose), carboxylic acid buffers (citric, tartaric, malic, and acetic) and an amino acid buffer (histidine HCl) were studied. Aqueous solutions of buffers, lyoprotectants and mixtures of the two were cooled from room temperature to -20°C and sonicated to induce solute crystallization. The crystallized phases were identified by X-ray diffractometry (laboratory or synchrotron source). Sonication accelerated crystallization of trehalose dihydrate in frozen trehalose solutions. Sonication also enhanced solute crystallization in tartaric (200 mM; pH 5), citric (200 mM pH 4) and malic (200 mM; pH 4) acid buffers. At lower buffer concentrations, longer annealing times following sonication were required to facilitate solute crystallization. The time for crystallization of histidine HCl progressively increased as a function of sucrose concentration. The insonation period required to effect crystallization also increased with sucrose concentration. Sonication can substantially accelerate solute crystallization in the freeze-concentrate. Ultrasonication may be useful in assessing the crystallization tendency of formulation constituents used in long term frozen storage and freeze-drying.

Crystal structure, spectral, thermal and dielectric studies of a new zinc benzoate single crystal

NASA Astrophysics Data System (ADS)

Bijini, B. R.; Prasanna, S.; Deepa, M.; Nair, C. M. K.; Rajendra Babu, K.

2012-11-01

Single crystals of zinc benzoate with a novel structure were grown in gel media. Sodium metasilicate of gel density 1.04 g/cc at pH 6 was employed to yield transparent single crystals. The crystal structure of the compound was ascertained by single crystal X-ray diffractometry. It was noted that the crystal belongs to monoclinic system with space group P21/c with unit cell parameters a = 10.669(1) Å, b = 12.995(5) Å, c = 19.119(3) Å, and β = 94.926(3)°. The crystal was seen to possess a linear polymeric structure along b-axis; with no presence of coordinated or lattice water. CHN analysis established the stoichiometric composition of the crystal. The existence of functional groups present in the single crystal system was confirmed by FT-IR studies. The thermal characteristic of the sample was analysed by TGA-DTA techniques, and the sample was found to be thermally stable up to 280 °C. The kinetic and thermodynamic parameters were also determined. UV-Vis spectroscopy corroborated the transparency of the crystal and revealed the optical band gap to be 4 eV. Dielectric studies showed decrease in the dielectric constant of the sample with increase in frequency.

World's Largest Gold Crystal Studied at Los Alamos

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

Vogel, Sven; Nakotte, Heinz

2014-04-03

When geologist John Rakovan needed better tools to investigate whether a dazzling 217.78-gram piece of gold was in fact the world's largest single-crystal specimen - a distinguishing factor that would not only drastically increase its market value but also provide a unique research opportunity - he traveled to Los Alamos National Laboratory's Lujan Neutron Scattering Center to peer deep inside the mineral using neutron diffractometry. Neutrons, different from other probes such as X-rays and electrons, are able to penetrate many centimeters deep into most materials. Revealing the inner structure of a crystal without destroying the sample - imperative, as thismore » one is worth an estimated $1.5 million - would allow Rakovan and Lujan Center collaborators Sven Vogel and Heinz Nakotte to prove that this exquisite nugget, which seemed almost too perfect and too big to be real, was a single crystal and hence a creation of nature. Its owner, who lives in the United States, provided the samples to Rakovan to assess the crystallinity of four specimens, all of which had been found decades ago in Venezuela.« less

World's Largest Gold Crystal Studied at Los Alamos

ScienceCinema

Vogel, Sven; Nakotte, Heinz

2018-02-07

When geologist John Rakovan needed better tools to investigate whether a dazzling 217.78-gram piece of gold was in fact the world's largest single-crystal specimen - a distinguishing factor that would not only drastically increase its market value but also provide a unique research opportunity - he traveled to Los Alamos National Laboratory's Lujan Neutron Scattering Center to peer deep inside the mineral using neutron diffractometry. Neutrons, different from other probes such as X-rays and electrons, are able to penetrate many centimeters deep into most materials. Revealing the inner structure of a crystal without destroying the sample - imperative, as this one is worth an estimated $1.5 million - would allow Rakovan and Lujan Center collaborators Sven Vogel and Heinz Nakotte to prove that this exquisite nugget, which seemed almost too perfect and too big to be real, was a single crystal and hence a creation of nature. Its owner, who lives in the United States, provided the samples to Rakovan to assess the crystallinity of four specimens, all of which had been found decades ago in Venezuela.

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

NASA Astrophysics Data System (ADS)

Jacques, Alain

2016-12-01

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

Alkyl group effects on CO insertion into coordinatively unsaturated early-transition-metal alkyls. Preparations and the first structural characterizations of tantalum enolate-O and tantalum. eta. sup 2 -acyl complexes

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

Meyer, T.Y.; Garner, L.R.; Baenziger, N.C.

1990-10-03

Low-pressure carbonylation of the mono(peralkylcyclopentadienyl)tantalum(V) alkyls ({eta}-C{sub 5}Me{sub 4}R)TaR{prime}Cl{sub 3} (R = Me, Et; R{prime} = CH{sub 2}C{sub 6}H{sub 4}-p-Me, CH{sub 2}CMe{sub 3}) yields either the O-bound enolate or the {eta}{sup 2}-acyl as shown by ir/NMR spectroscopy and x-ray diffractometry. The p-tolyl enolate ({eta}-C{sub 5}Me{sub 5})Ta(OCH{double bond}CHC{sub 6}H{sub 4}-p-Me)Cl{sub 3}, derived directly from carbonylation of the tantalum 4-methylbenzyl precursor, is shown to possess a cis configuration in solution and in the solid state. Key structural features from a single-crystal x-ray diffraction study of the tetrahydrofuran-ligated enolate complex are reported. The mechanism of formation of the enolate from carbonylation of themore » 4-methylbenzyl complex is discussed. The previously reported acyl ({eta}-C{sub 5}Me{sub 4}R)Ta(C(O)CH{sub 2}CMe{sub 3})Cl{sub 3} has been reexamined and found to possess a symmetric, strongly distorted {eta}{sup 2}-acyl coordination by solution {sup 1}H NMR spectroscopy and solid-state x-ray diffractometry. The molecular structures of ({eta}-C{sub 5}Me{sub 5})Ta(OCH{double bond}CHC{sub 6}H{sub 4}-p-Me)Cl{sub 3} and ({eta}-C{sub 5}Me{sub 5})Ta(C(O)CH{sub 2}CMe{sub 3})Cl{sub 3}, which are reported here, are the first structural determinations of a tantalum enolate and of a tantalum {eta}{sup 2}-acyl. 41 refs., 2 figs., 8 tabs.« less

Role of the Strength of Drug-Polymer Interactions on the Molecular Mobility and Crystallization Inhibition in Ketoconazole Solid Dispersions.

PubMed

Mistry, Pinal; Mohapatra, Sarat; Gopinath, Tata; Vogt, Frederick G; Suryanarayanan, Raj

2015-09-08

The effects of specific drug-polymer interactions (ionic or hydrogen-bonding) on the molecular mobility of model amorphous solid dispersions (ASDs) were investigated. ASDs of ketoconazole (KTZ), a weakly basic drug, with each of poly(acrylic acid) (PAA), poly(2-hydroxyethyl methacrylate) (PHEMA), and polyvinylpyrrolidone (PVP) were prepared. Drug-polymer interactions in the ASDs were evaluated by infrared and solid-state NMR, the molecular mobility quantified by dielectric spectroscopy, and crystallization onset monitored by differential scanning calorimetry (DSC) and variable temperature X-ray diffractometry (VTXRD). KTZ likely exhibited ionic interactions with PAA, hydrogen-bonding with PHEMA, and weaker dipole-dipole interactions with PVP. On the basis of dielectric spectroscopy, the α-relaxation times of the ASDs followed the order: PAA > PHEMA > PVP. In addition, the presence of ionic interactions also translated to a dramatic and disproportionate decrease in mobility as a function of polymer concentration. On the basis of both DSC and VTXRD, an increase in strength of interaction translated to higher crystallization onset temperature and a decrease in extent of crystallization. Stronger drug-polymer interactions, by reducing the molecular mobility, can potentially delay the crystallization onset temperature as well as crystallization extent.

Clay-mineraloid weathering products in Antarctic meteorites

NASA Technical Reports Server (NTRS)

Gooding, James L.

1986-01-01

The production of clay mineraloids (CMs) in the weathering of stony meteorites recovered in the Allan Hills and Elephant Moraine areas of Antarctica is investigated, applying electron microbeam analysis, pyrolysis/mass spectroscopy, X-ray diffractometry, and differential scanning calorimetry to whole-rock chips from two eucrites, two diogenites, and an H5 chondrite. The data are presented in tables, graphs, and photomicrographs and characterized in detail. Massive to incipient-vermicular CM formations with smectitelike or micalike compositions and indications of poor crystallization are observed and attributed to hydrocryogenic diagenesis (with little or no liquid water) on time scales of 10-1000 kyr. The need to take the compositional effects of weathering into account before attempting to reconstruct the preterrestrial histories of meteorites is stressed.

An epistemology on the nature of polymers.

PubMed

Laridjani, Mortéza; Leboucher, Pierre

2014-01-01

Liquids have neither a periodic structure nor the completely random character of gases therefore the detailed study of their x-ray scattering diagram encounters many difficulties. The idea of periodic regularity in molecules of liquid polymers has been an attractive proposition for the simple interpretation of liquid polymer x-ray diagrams. The categorisation of polymer substances as being between a crystal phase with a perfect order and an amorphous disordered state is an over simplification of the complex reality. For obtaining structural information, during the early stages of the application of x-ray diffraction, a near crystalline model of the molecular arrangements in liquids was utilised. However, the results from these investigations led to just an approximation of the crystalline state. Our studies have analysed the real image of Fourier space of liquid polymers, for the first time, using anomalous diffractometry. The findings show the precise atomic structure of liquid polymers when transformed, by cooling, to solid polymers. We demonstrate that there is an intermediate ordered structure, characterised by the real full image of Fourier space. This prominent state of matter, an intermediate ordered structure, is defined by a regular unit cell with a five-fold symmetry. These structural atomic studies contribute to a more detailed understanding of the properties of polymers than the traditional studies of the degree of crystallinity.

An Epistemology on the Nature of Polymers

PubMed Central

Laridjani, Mortéza; Leboucher, Pierre

2014-01-01

Liquids have neither a periodic structure nor the completely random character of gases therefore the detailed study of their x-ray scattering diagram encounters many difficulties. The idea of periodic regularity in molecules of liquid polymers has been an attractive proposition for the simple interpretation of liquid polymer x-ray diagrams. The categorisation of polymer substances as being between a crystal phase with a perfect order and an amorphous disordered state is an over simplification of the complex reality. For obtaining structural information, during the early stages of the application of x-ray diffraction, a near crystalline model of the molecular arrangements in liquids was utilised. However, the results from these investigations led to just an approximation of the crystalline state. Our studies have analysed the real image of Fourier space of liquid polymers, for the first time, using anomalous diffractometry. The findings show the precise atomic structure of liquid polymers when transformed, by cooling, to solid polymers. We demonstrate that there is an intermediate ordered structure, characterised by the real full image of Fourier space. This prominent state of matter, an intermediate ordered structure, is defined by a regular unit cell with a five-fold symmetry. These structural atomic studies contribute to a more detailed understanding of the properties of polymers than the traditional studies of the degree of crystallinity. PMID:25329440

Complete p-type activation in vertical-gradient freeze GaAs co-implanted with gallium and carbon

NASA Astrophysics Data System (ADS)

Horng, S. T.; Goorsky, M. S.

1996-03-01

High-resolution triple-axis x-ray diffractometry and Hall-effect measurements were used to characterize damage evolution and electrical activation in gallium arsenide co-implanted with gallium and carbon ions. Complete p-type activation of GaAs co-implanted with 5×1014 Ga cm-2 and 5×1014 C cm-2 was achieved after rapid thermal annealing at 1100 °C for 10 s. X-ray diffuse scattering was found to increase after rapid thermal annealing at 600-900 °C due to the aggregation of implantation-induced point defects. In this annealing range, there was ˜10%-72% activation. After annealing at higher annealing temperatures, the diffuse scattered intensity decreased drastically; samples that had been annealed at 1000 °C (80% activated) and 1100 °C (˜100% activated) exhibited reciprocal space maps that were indicative of high crystallinity. The hole mobility was about 60 cm2/V s for all samples annealed at 800 °C and above, indicating that the crystal perfection influences dopant activation more strongly than it influences mobility. Since the high-temperature annealing simultaneously increases dopant activation and reduces x-ray diffuse scattering, we conclude that point defect complexes which form at lower annealing temperatures are responsible for both the diffuse scatter and the reduced activation.

Predicting the crystallization propensity of carboxylic acid buffers in frozen systems--relevance to freeze-drying.

PubMed

Sundaramurthi, Prakash; Suryanarayanan, Raj

2011-04-01

Selective crystallization of buffer components in frozen solutions is known to cause pronounced pH shifts. Our objective was to study the crystallization behavior and the consequent pH shift in frozen aqueous carboxylic acid buffers. Aqueous carboxylic acid buffers were cooled to -25°C and the pH of the solution was measured as a function of temperature. The thermal behavior of solutions during freezing and thawing was investigated by differential scanning calorimetry. The crystallized phases in frozen solution were identified by X-ray diffractometry. The malate buffer system was robust with no evidence of buffer component crystallization and hence negligible pH shift. In the citrate and tartarate systems, at initial pH

Impacts of compression on crystallization behavior of freeze-dried amorphous sucrose.

PubMed

Imamura, Koreyoshi; Nomura, Mayo; Tanaka, Kazuhiro; Kataoka, Nobuhide; Oshitani, Jun; Imanaka, Hiroyuki; Nakanishi, Kazuhiro

2010-03-01

An amorphous matrix comprised of sugar molecules is used as excipient and stabilizing agent for labile ingredients in the pharmaceutical industry. The amorphous sugar matrix is often compressed into a tablet form to reduce the volume and improve handling. Herein, the effect of compression on the crystallization behavior of an amorphous sucrose matrix was investigated. Amorphous sucrose samples were prepared by freeze-drying and compressed under different conditions, followed by analyses by differential scanning calorimetry, isothermal crystallization tests, X-ray powder diffractometry, Fourier transform infrared spectroscopy (FTIR), and gas pycnometry. The compressed sample had a lower crystallization temperature and a shorter induction period for isothermal crystallization, indicating that compression facilitates the formation of the critical nucleus of a sucrose crystal. Based on FTIR and molecular dynamics simulation results, the conformational distortion of sucrose molecules due to the compression appears to contribute to the increase in the free energy of the system, which leads to the facilitation of critical nucleus formation. An isothermal crystallization test indicated an increase in the growth rate of sucrose crystals by the compression. This can be attributed to the transformation of the microstructure from porous to nonporous, as the result of compression. 2009 Wiley-Liss, Inc. and the American Pharmacists Association

Structural properties of ultrafine Ba-hexaferrite nanoparticles

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

Makovec, Darko, E-mail: Darko.Makovec@ijs.si; Primc, Darinka; Sturm, Saso

2012-12-15

Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was studied using X-ray diffractometry (XRD), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDXS), X-ray absorption fine structure (XAFS), and Moessbauer spectroscopy (MS), to be compared to the structure of larger nanoparticles and the bulk. The nanoparticles were synthesized with hydrothermal treatment of an appropriate suspension of Ba and Fe hydroxides in the presence of a large excess of OH{sup -}. The ultrafine nanoparticles were formed in a discoid shape, {approx}10 nm wide and only {approx}3 nm thick, comparable to the size of the hexagonal unit cell in the c-direction.more » The HRTEM image analysis confirmed the hexaferrite structure, whereas EDXS showed the composition matching the BaFe{sub 12}O{sub 19} formula. XAFS and MS analyses showed considerable disorder of the structure, most probably responsible for the low magnetization. - Graphical abstract: Left: HREM image of an ultrafine Ba-hexaferrite nanoparticle (inset: TEM image of the nanoparticles); Right: the experimental HRTEM image is compared with calculated image and corresponding atomic model. Highlights: Black-Right-Pointing-Pointer Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was compared to the structure of the bulk. Black-Right-Pointing-Pointer Thickness the discoid nanoparticles was comparable to the size of the hexagonal unit cell in the c-direction. Black-Right-Pointing-Pointer Considerable disorder of the nanoparticles' structure is most probably responsible for their low magnetization.« less

Structural changes concurrent with ferromagnetic transition

NASA Astrophysics Data System (ADS)

Yang, Sen; Bao, Hui-Xin; Zhou, Chao; Wang, Yu; Ren, Xiao-Bing; Song, Xiao-Ping; Yoshitaka, Matsushita; Yoshio, Katsuya; Masahiko, Tanaka; Keisuke, Kobayashi

2013-04-01

Ferromagnetic transition has generally been considered to involve only an ordering of magnetic moment with no change in the host crystal structure or symmetry, as evidenced by a wealth of crystal structure data from conventional X-ray diffractometry (XRD). However, the existence of magnetostriction in all known ferromagnetic systems indicates that the magnetic moment is coupled to the crystal lattice; hence there is a possibility that magnetic ordering may cause a change in crystal structure. With the development of high-resolution synchrotron XRD, more and more magnetic transitions have been found to be accompanied by simultaneous structural changes. In this article, we review our recent progress in understanding the structural change at a ferromagnetic transition, including synchrotron XRD evidence of structural changes at the ferromagnetic transition, a phenomenological theory of crystal structure changes accompanying ferromagnetic transitions, new insight into magnetic morphotropic phase boundaries (MPB) and so on. Two intriguing implications of non-centric symmetry in the ferromagnetic phase and the first-order nature of ferromagnetic transition are also discussed here. In short, this review is intended to give a self-consistent and logical account of structural change occurring simultaneously with a ferromagnetic transition, which may provide new insight for developing highly magneto-responsive materials.

Uncommon and Emissive {[Au2(C3H6NS2)2][Au(C3H6NS2)2]2(PF6)2} Mixed Au+ and Au3+ Pseudotetranuclear Crystalline Compound: Synthesis, Structural Characterization, and Optical Properties.

PubMed

Langaro, Ana P; Souza, Ana K R; Morassuti, Claudio Y; Lima, Sandro M; Casagrande, Gleison A; Deflon, Victor M; Nunes, Luiz A O; Da Cunha Andrade, Luis H

2016-11-23

An uncommon emissive pseudotetranuclear compound, {[Au 2 (C 3 H 6 NS 2 ) 2 ][Au(C 3 H 6 NS 2 ) 2 ] 2 (PF 6 ) 2 }, was synthesized and characterized in terms of its structure and optical properties. The synthesis produced a crystalline compound composed of four gold atoms with two different oxidation states (Au + and Au 3+ ) in the same crystalline structure. The title complex belonged to a triclinic crystalline system involving the centrosymmetric P1̅ space group. X-ray diffractometry and vibrational spectroscopy (infrared, Raman, and SERS) were used for structural characterization of the new crystal. The vibrational spectroscopy techniques supported the X-ray diffraction results and confirmed the presence of bonds including Au-Au and Au-S. Optical characterization performed using UV-vis spectroscopy showed that under ultraviolet excitation, the emissive crystalline complex presented characteristic broad luminescent bands centered at 420 and 670 nm.

Xylitol as a potential co-crystal co-former for enhancing dissolution rate of felodipine: preparation and evaluation of sublingual tablets.

PubMed

Arafa, Mona F; El-Gizawy, Sanaa A; Osman, Mohamed A; El Maghraby, Gamal M

2018-06-01

Dissolution enhancement is a promising strategy for improving drug bioavailability. Co-crystallization of drugs with inert material can help in this direction. The benefit will become even greater if the inert material can form co-crystal while maintaining its main function as excipient. Accordingly, the objective of the current study was to investigate xylitol as a potential co-crystal co-former for felodipine with the goal of preparing felodipine sublingual tablets. Co-crystallization was achieved by wet co-grinding of the crystals deposited from methanolic solutions containing felodipine with increasing molar ratios of xylitol (1:1, 1:2 and 1:3). The developed co-crystals were characterized using Fourier transform infrared spectroscopy (FTIR), X-ray diffractometry (XRD), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) before monitoring drug dissolution. These results reflected the development of new crystalline species depending on the relative proportions of felodipine and xylitol with complete co-crystallization of felodipine being achieved in the presence of double its molar concentration of xylitol. This co-crystal formulation was compressed into sublingual tablet with ultrashort disintegration time with subsequent fast dissolution. Co-crystal formation was associated with enhanced dissolution with the optimum formulation producing the fastest dissolution rate. In conclusion, xylitol can be considered as a co-crystal co-former for enhanced dissolution rate of drugs.

Synthesis of Copper-Antimony-Sulfide Nanocrystals for Solution-Processed Solar Cells.

PubMed

Suehiro, Satoshi; Horita, Keisuke; Yuasa, Masayoshi; Tanaka, Tooru; Fujita, Katsuhiko; Ishiwata, Yoichi; Shimanoe, Kengo; Kida, Tetsuya

2015-08-17

The p-type nanocrystals (NCs) of copper-based chalcogenides, such as CuInSe2 and Cu2ZnSnS4, have attracted increasing attention in photovoltaic applications due to their potential to produce cheap solution-processed solar cells. Herein, we report the synthesis of copper-antimony-sulfide (CAS) NCs with different crystal phases including CuSbS2, Cu3SbS4, and Cu12Sb4S13. In addition, their morphology, crystal phase, and optical properties were characterized using transmission electron microscopy, X-ray diffractometry, UV-vis-near-IR spectroscopy, and photoemission yield spectroscopy. The morphology, crystal phase, and electronic structure were significantly dependent on the chemical composition in the CAS system. Devices were fabricated using particulate films consisting of CAS NCs prepared by spin coating without a high-temperature treatment. The CAS NC-based devices exhibited a diode-like current-voltage characteristic when coupled with an n-type CdS layer. In particular, the CuSbS2 NC devices exhibited photovoltaic responses under simulated sunlight, demonstrating its applicability for use in solution-processed solar cells.

[Effect of crystallization temperature of palm oil on its crystallization. IV. The influence of tripalmitoylglycerol (PPP) on the crystallization of 1,3-dipalmitoyl-2-oleoyl-glycerol (POP) and 1,2-dioleoyl-3-palmitoyl-glycerol (POO)].

PubMed

Mihara, Hiroaki; Ishiguro, Takashi; Fukano, Hidenori; Taniuchi, Shigeyuki; Ogino, Keizo

2007-01-01

Triacylglycerin in Palm Oil contains POP (1,3-dipalmitoyl-2-oleoyl-glycerol) at 30%, POO (1,2-dioleoyl-3-palmitoyl-glycerol) at 20% and PPP (tripalmitoylglycerol) at 5%. The crystallization temperature of PPP is high and the rates of crystal nuclear formation and growth are fast. It is thus considered that PPP may have some effect on the manner or mode of Palm Oil. Examination was thus made to clarify how PPP may affect the crystallization of POP and POO by differential scanning calorimetry (DSC) and X ray diffractometry (XRD) conducted on PPP/POP and PPP/POO mixtures. High and low temperature peaks were noted to appear on the DSC crystallization curve for either of these mixtures. The high temperature peak was considered possibly due to PPP, and the low temperature peak, to POP or POO. DSC isothermal analysis indicated the rate of crystal growth of either mixture to exceed that of pure of POP or POO. Crystal mixture structure was also seen to be complicated than either compound in pure form. The present findings thus clearly indicate that clarification should be made of the effects of high melting point triacylglycerin, such as PPP, on the crystallization of Palm Oil.

Controlling the physical form of mannitol in freeze-dried systems.

PubMed

Mehta, Mehak; Bhardwaj, Sunny P; Suryanarayanan, Raj

2013-10-01

A potential drawback with the use of mannitol as a bulking agent is its existence as mannitol hemihydrate (MHH; C₆H₁₄O₆·0.5H₂O) in the lyophile. Once formed during freeze-drying, MHH dehydration may require secondary drying under aggressive conditions which can be detrimental to the stability of thermolabile components. If MHH is retained in the lyophile, the water released by MHH dehydration during storage has the potential to cause product instability. We systematically identified the conditions under which anhydrous mannitol and MHH crystallized in frozen systems with the goal of preventing MHH formation during freeze-drying. When mannitol solutions were cooled, the temperature of solute crystallization was the determinant of the physical form of mannitol. Based on low temperature X-ray diffractometry (using both laboratory and synchrotron sources), MHH formation was observed when solute crystallization occurred at temperatures ≤ -20 °C, while anhydrous mannitol crystallized at temperatures ≤ -10 °C. The transition temperature (anhydrate - MHH) appears to be ∼-15 °C. The use of a freeze-dryer with controlled ice nucleation technology enabled anhydrous mannitol crystallization at ∼-5 °C. Thus, ice crystallization followed by annealing at temperatures ≤ -10 °C can be an effective strategy to prevent MHH formation. Copyright © 2013 Elsevier B.V. All rights reserved.

Relation between the structural parameters of metallic glasses at the onset crystallization temperatures and threshold values of the effective diffusion coefficients

NASA Astrophysics Data System (ADS)

Tkatch, V. I.; Svyrydova, K. A.; Vasiliev, S. V.; Kovalenko, O. V.

2017-08-01

Using the results of differential scanning calorimetry and X-ray diffractometry, an analysis has been carried out of the initial stages of the eutectic and primary mechanisms of crystallization of a series of metallic glasses based on Fe and Al with the established temperature dependences of the effective diffusion coefficients. Analytical relationships, which relate the volume density of crystallites formed in the glasses at the temperatures of the onset of crystallization with the values of the effective diffusion coefficients at these temperatures have been proposed. It has been established that, in the glasses, the crystallization of which begins at the lower boundary of the threshold values of the effective diffusion coefficients ( 10-20 m2/s), structures are formed with the volume density of crystallites on the order of 1023-1024 m-3 and, at the upper boundary (10-18 m2/s), of the order of 1018 and 1020 m-3 in the glasses that are crystallized via the eutectic and primary mechanisms, respectively. Good agreement between the calculated and experimental estimates indicates that the threshold values of the effective diffusion coefficients are the main factors that determine the structure of glasses at the initial stages of crystallization.

Method for improve x-ray diffraction determinations of residual stress in nickel-base alloys

DOEpatents

Berman, Robert M.; Cohen, Isadore

1990-01-01

A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys which comprises covering part of a predetermined area of the surface of a nickel-base alloy with a dispersion, exposing the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample.

Synthesis of core-shell structured FAU/SBA-15 composite molecular sieves and their performance in catalytic cracking of polystyrene

NASA Astrophysics Data System (ADS)

Du, Jinlong; Shi, Chunwei; Wu, Wenyuan; Bian, Xue; Chen, Ping; Cui, Qingzhu; Cui, Zhixuan

2017-12-01

Composite molecular sieves, FAU/SBA-15, having core-shell structure were synthesized. The synthesized composite sieves were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), pyrolysis fourier transform infrared (Py-FTIR) spectroscopy, temperature programmed desorption spectra (NH3-TPD), UV Raman spectroscopy, nuclear magnetic resonance (NMR) and other techniques. XRD, SEM, TEM, N2 adsorption-desorption, mass spectrometry, NMR and EDS results showed that the composite molecular sieve contained two pore channels. Py-FTIR results showed that the addition of HY molecular sieves improved the acidity of the composite zeolite. The crystallization mechanism during the growth of FAU/SBA-15 shell was deduced from the influence of crystallization time on the synthesis of FAU/SBA-15 core-shell structured composite molecular sieve. HY dissociated partially in H2SO4 solution, and consisted of secondary structural units. This framework structure was more stable than its presence in the isolated form on the same ring or in the absence of Al. Thus it played a guiding role and connected with SBA-15 closely through the Si-O bond. This resulted in the gradual covering of the exterior surface of FAU phase by SBA-15 molecular sieves. The presence of SBA-15 restricted the formation of the other high mass components and increased the selectivity towards ethylbenzene.

Lattice damage and Al-metal precipitation in 2.5 MeV-electron-irradiated AlH3

NASA Astrophysics Data System (ADS)

Zogal, O. J.; Vajda, P.; Beuneu, F.; Pietraszko, A.

1998-04-01

AlH3 powder was bombarded with energetic electrons at 20 K and at room temperature and investigated by EPR, NMR, X-ray diffractometry, and microwave dielectric-constant measurements. The EPR spectra of the irradiated powder and of a selected single crystal cuboid of ˜ {10^{ - 1}} mm edge show a complex asymmetric line centered at g = 2.009, with a Curie-like temperature dependence, attributed to radiation-induced color centers and/or their agglomerates. At the same time, the grains, which have become shiny black after irradiation, exhibit an increase of both the real and the imaginary part of ɛ. 27Al-NMR spectra of the irradiated powder present a Knight-shifted line at 1600(50) ppm, close to the position of bulk metallic Al, and corresponding to a concentration of c(Al) ˜ {10^{ - 1}}. In addition, the main hydride line differs from that before irradiation, demonstrating an alteration of environmental symmetry. The irradiation induces also a change in shape and width of the 1H-NMR line, another indication of symmetry change in the lattice. Finally, a refined X-ray single-crystal structure analysis of the irradiated cuboid indicates a change of structure from trigonal R -3 c to R -3, with a loss of mirror symmetry for the two Al sites caused by the introduction of Al-defects in the vicinity of one of them.

A Solid-State NMR Study of Selenium Substitution into Nanocrystalline Hydroxyapatite

PubMed Central

Kolmas, Joanna; Kuras, Marzena; Oledzka, Ewa; Sobczak, Marcin

2015-01-01

The substitution of selenium oxyanions in the hydroxyapatite structure was examined using multinuclear solid-state resonance spectroscopy (ssNMR). The study was supported by powder X-ray diffractometry (PXRD) and wavelength dispersion X-ray fluorescence (WD-XRF). Samples of pure hydroxyapatite (HA300) and selenate (HA300-1.2SeO4) or selenite (HA300-1.2SeO3) substituted hydroxyapatites were synthesized using the standard wet method and heated at 300 °C to remove loosely bonded water. PXRD data showed that all samples are single-phase, nanocrystalline hydroxyapatite. The incorporation of selenite and selenate ions affected the lattice constants. In selenium-containing samples the concentration of Se was very similar and amounted to 9.55% and 9.64%, for HA300-1.2SeO4 and HA300-1.2SeO3, respectively. PXRD and ssNMR data showed that the selenite doping significantly decreases the crystallite size and crystallinity degree. 31P and 1H NMR experiments demonstrated the developed surface hydrated layer in all samples, especially in HA300-1.2SeO3. 1H NMR studies showed the dehydroxylation of HA during the selenium oxyanions substitution and the existence of hydrogen bonding in structural hydroxyl group channels. 1H→77Se cross polarization NMR experiments indicated that selenites and selenates are located in the crystal lattice and on the crystal surface. PMID:25997001

Morphology and structure features of ZnAl{sub 2}O{sub 4} spinel nanoparticles prepared by matrix-isolation-assisted calcination

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

Du, Xuelian, E-mail: xueliandu@126.com; Li, Liqiang; Zhang, Wenxing

2015-01-15

Graphical abstract: The substrate ZnO as the isolation medium is effective in preventing the sintering and agglomeration of ZnAl{sub 2}O{sub 4} nanoparticles, and it also prevents their contamination. High purity, well-dispersed, and single-crystal ZnAl{sub 2}O{sub 4} nanoparticles with 3.72 eV band gap were obtained. - Abstract: Well-dispersed ZnAl{sub 2}O{sub 4} spinel nanoparticles with an average crystalline size of 25.7 nm were synthesized successfully and easily by polymer-network and matrix-isolation-assisted calcination. The product microstructure and features were investigated by X-ray diffractometry, thermogravimetric and differential thermal analysis, Fourier transform-infrared spectroscopy, N{sub 2} adsorption–desorption isotherms, and energy dispersive X-ray spectra. The morphology andmore » optical performance of the as-prepared ZnAl{sub 2}O{sub 4} nanoparticles were characterized by scanning electron microscope, transmission electron microscopy, and photoluminescence spectrometer. Experimental results indicate that excess ZnO acted as the isolation medium is effective in preventing the sintering and agglomeration of ZnAl{sub 2}O{sub 4} nanoparticles, and it also prevents their contamination. Then, high purity and well-dispersed ZnAl{sub 2}O{sub 4} nanoparticles with single-crystal structure were obtained.« less

The solid state of rebamipide: preparation, characterization, and dissolution.

PubMed

Jeon, Seong Hyeon; Sohn, Young Taek

2016-04-01

Rebamipide is marketed as a peptic ulcer agent under the trade name Mucosta(R). The objective of this work was to investigate the existence of polymorphs and pseudopolymorphs of rebamipide. Two crystal forms of rebamipide were isolated by recrystallization and characterized by differential thermal analysis (DTA), thermogravimetric analysis (TG), powder X-ray diffractometry, infrared spectrometry, and nuclear magnetic resonance. The DTA curve of Form 1 showed one endothermic peak at 305.2 °C, and that of Form 2 showed one endothermic peak at 307.3 °C. The TG curve of Form 1 showed a single weight loss at 305.2 °C, which corresponded to melting. The TG curve of Form 2 also showed a single weight loss at 307.3 °C, which corresponded to melting. The melting point of Form 2 was higher than that of Form 1. In the dissolution studies in pH 6.8 buffer at 37 ± 0.5 °C, the two crystal forms showed no significant differences in dissolution. After 3 months of storage at 0, 52, and 95% RH, the two crystal forms were not transformed. After milling with a Specamill for 2 h, the two crystal forms were not transformed.

Synthesis, Crystal Structure, and Magnetic Properties of the YbFeTi2O7 Compound

NASA Astrophysics Data System (ADS)

Drokina, T. V.; Petrakovskii, G. A.; Molokeev, M. S.; Velikanov, D. A.

2018-03-01

We report on the synthesis conductions and results of experimental investigations of the crystal structure and magnetic properties of a new magnetic compound YbFeTi2O7. According to the X-ray diffractometry data, the crystal structure of the investigated compound is described by the rhombic space group Pcnb with unit cell parameters of a = 9.8115(1) Å, b = 13.5106(2) Å, and c = 7.31302(9) Å and atomic disordering in the distribution of iron ions Fe3+ over five structural sites. The magnetic measurements in the lowtemperature region revealed a kink in the temperature dependence of the magnetic moment and its dependence on the sample magnetic prehistory. The experimental results obtained suggest that with a decrease in temperature the sample passes from the paramagnetic state to the spin-glass-like magnetic state characterized by a freezing temperature of T f = 4.5 K at the preferred antiferromagnetic exchange coupling in the sample spin system. The chemical pressure variation upon replacement of rare-earth ion R by Yb in the RFeTi2O7 system does not change the crystal lattice symmetry and magnetic state.

Concave Urinary Crystallines: Direct Evidence of Calcium Oxalate Crystals Dissolution by Citrate In Vivo

PubMed Central

Shang, Yun-Feng; Xu, Meng; Zhang, Guang-Na; Ouyang, Jian-Ming

2013-01-01

The changes in urinary crystal properties in patients with calcium oxalate (CaOx) calculi after oral administration of potassium citrate (K3cit) were investigated via atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray powder diffractometry (XRD), and zeta potential analyzer. The AFM and SEM results showed that the surface of urinary crystals became concave, the edges and corners of crystals became blunt, the average size of urinary crystallines decreased significantly, and aggregation of urinary crystals was reduced. These changes were attributed to the significant increase in concentration of excreted citrate to 492 ± 118 mg/L after K3cit intake from 289 ± 83 mg/L before K3cit intake. After the amount of urinary citrate was increased, it complexed with Ca2+ ions on urinary crystals, which dissolved these crystals. Thus, the appearance of concave urinary crystals was a direct evidence of CaOx dissolution by citrate in vivo. The XRD results showed that the quantities and species of urinary crystals decreased after K3cit intake. The mechanism of inhibition of formation of CaOx stones by K3cit was possibly due to the complexation of Ca2+ with citrate, increase in urine pH, concentration of urinary inhibitor glycosaminoglycans (GAGs), and the absolute value of zeta potential after K3cit intake. PMID:24363634

Anisotropic magnetic properties of the KMo4O6

NASA Astrophysics Data System (ADS)

Andrade, M.; Maffei, M. L.; Dos Santos, C. A. M.; Ferreira, B.; Sartori, A. F.

2012-02-01

Electrical resistivity measurements in the tetragonal KMo4O6 single crystals show a metal-insulator transition (MIT) near 100K. Magnetization measurements as a function of temperature show no evidence of magnetic ordering at this MIT [1]. Single crystals of KMo4O6 were obtained by electrolysis of a melt with a molar ratio of K2MoO4:MoO3 = 6:1. The process were carried out at 930 C with a current of 20-25mA for 52h in argon atmosphere. After that, electrodes were removed from the melt alloying the crystals to cool down to room temperature rapidly. Scanning Electron Microscopy (SEM) showed that the black single crystals were grown on the platinum cathode. Typical dimensions of the single crystals are 1x0.2x0.2mm^3. X-ray diffractometry confirmed that the single crystals have KMo4O6 tetragonal crystalline structure with space group P4. Magnetization measurements were performed parallel and perpendicular to the c-axis from 2 to 300K. The results show anisotropic behavior between both directions. Furthermore, the temperature independence of the magnetization at high temperature and the upturn at low temperature are observed in agreement with previous results [1]. MxH curves measured at several temperatures show nonlinear behavior and a small magnetic ordering. The magnetic ordering seems to be related to the MIT near 100K. This material is based upon support by FAPESP (2009/14524-6 and 2009/54001-6) and CNPq/NSF (490182/2009-7). M. Andrade is CAPES fellow and C.A.M. dos Santos is CNPq fellow. [4pt] [1] K. V. Ramanujachary et al., J. Sol. State Chem.102 (1993) 69.

Processing of copper converter slag for metals reclamation: Part II: mineralogical study.

PubMed

Deng, Tong; Ling, Yunhan

2004-10-01

Chemical and mineralogical characterizations of a copper converter slag, and its products obtained by curing with strong sulphuric acid and leaching with hot water, were carried out using ore microscopy, scanning electronic microscopy with energy dispersive spectrometry, wave-length dispersive X-ray fluorescence spectrometry, X-ray diffractometry and chemical phase analysis, which provided necessary information to develop a new process for treating such slag and further understanding of the chemical and mineralogical changes in the process.

Investigations on nucleation, HRXRD, optical, piezoelectric, polarizability and Z-scan analysis of L-arginine maleate dihydrate single crystals

NASA Astrophysics Data System (ADS)

Sakthy Priya, S.; Alexandar, A.; Surendran, P.; Lakshmanan, A.; Rameshkumar, P.; Sagayaraj, P.

2017-04-01

An efficient organic nonlinear optical single crystal of L-arginine maleate dihydrate (LAMD) has been grown by slow evaporation solution technique (SEST) and slow cooling technique (SCT). The crystalline perfection of the crystal was examined using high-resolution X-ray diffractometry (HRXRD) analysis. Photoluminescence study confirmed the optical properties and defects level in the crystal lattice. Electromechanical behaviour was observed using piezoelectric co-efficient (d33) analysis. The photoconductivity analysis confirmed the negative photoconducting nature of the material. The dielectric constant and loss were measured as a function of frequency with varying temperature and vice-versa. The laser damage threshold (LDT) measurement was carried out using Nd:YAG Laser with a wavelength of 1064 nm (Focal length is 35 cm) and the obtained results showed that LDT value of the crystal is high compared to KDP crystal. The high laser damage threshold of the grown crystal makes it a potential candidate for second and higher order nonlinear optical device application. The third order nonlinear optical parameters of LAMD crystal is determined by open-aperture and closed-aperture studies using Z-scan technique. The third order linear and nonlinear optical parameters such as the nonlinear refractive index (n2), two photon absorption coefficient (β), Real part (Reχ3) and imaginary part (Imχ3) of third-order nonlinear optical susceptibility are calculated.

Biocompatibility of the micro-patterned NiTi surface produced by femtosecond laser

NASA Astrophysics Data System (ADS)

Liang, Chunyong; Wang, Hongshui; Yang, Jianjun; Li, Baoe; Yang, Yang; Li, Haipeng

2012-11-01

Biocompatibility of the micro-patterned NiTi surface produced by femtosecond laser (FSL) was studied in this work. The surface characteristics of the laser treated NiTi alloys were investigated by scanning electron microscopy (SEM), atom force microscopy (AFM), X-ray diffractometry (XRD) and X-ray photoelectron spectrum (XPS). The biocompatibility was evaluated by in vitro cell culture test. The results showed that, grooves, ripples, which covered by nanoparticles were formed on the sample surfaces, and the Ni/Ti ratio on the alloy surface increased with increasing laser energy. The crystal structure was not changed by laser treatment. However, the cell culture test proved that the micro-patterns induced by FSL were beneficial to improve the biocompatibility of NiTi alloys: the growth of osteoblasts oriented along the grooves, a large amount of synapses and filopodias were formed due to the ripples, holes and nanoparticles on the alloy surface, and the proliferation rate and alkaline phosphatase (ALP) content of cells were increased after FSL treatment. However, due to the toxicity of Ni ions on cell growth, the NiTi alloy surface should not be treated by laser fluence of more than 3.82 J/cm2 to obtain the ideal biocompatibility.

Preparation of MWCNT-Fe3O4 Nanocomposites from Iron Sand Using Sonochemical Route

NASA Astrophysics Data System (ADS)

Rahmawati, R.; Melati, A.; Taufiq, A.; Sunaryono; Diantoro, M.; Yuliarto, B.; Suyatman, S.; Nugraha, N.; Kurniadi, D.

2017-05-01

The composites of multi-walled carbon nanotube (MWCNT) and magnetite (Fe3O4) nanoparticles from iron sand were successfully prepared via the sonochemical route. In this experiment, the MWCNT-Fe3O4 nanocomposites were prepared with different compositions of MWCNT (0.01%, 0.02%, and 0.04%) with the constant composition of Fe3O4 particles. The characterizations were performed by means of X-Ray Diffractometry (XRD), Fourier Transform Infra-Red (FTIR) Spectrometer and Scanning Electron Microscopy (SEM) integrated with Energy Dispersive X-Ray (EDX). The XRD data analysis showed that the Fe3O4 crystallize in spinel structure in nanometric size. Furthermore, the crystallinity of the samples tended to reduce by increasing the MWCNT compositions. The SEM images showed that Fe3O4 tend to agglomerate in nanometric size. The FTIR spectra detected the functional groups of Fe-O bonding that showed the existence of Fe2+ and Fe3+. In the composites, the Fe3O4 nanoparticles were physically mixed with the MWCNTs constructing a unique structure. The as prepared MWCNT-Fe3O4 nanocomposites have the potential for bio-applications.

On the dynamics of water molecules at the protein solute interfaces.

PubMed

Bernini, A; Spiga, O; Ciutti, A; Chiellini, S; Menciassi, N; Venditti, V; Niccolai, N

2004-10-01

Proteins, with the large variety of chemical groups they present at their molecular surface, are a class of molecules which can be very informative on most of the possible solute-solvent interactions. Hen egg white lysozyme has been used as a probe to investigate the complex solvent dynamics occurring at the protein surface, by analysing the results obtained from Nuclear Magnetic Resonance, X-ray diffractometry and Molecular Dynamics simulations. A consistent overall picture for the dynamics of water molecules close to the protein is obtained, suggesting that a rapid exchange occurs, in a picosecond timescale, among all the possible hydration surface sites both in solution and the solid state, excluding the possibility that solvent molecules can form liquid-crystal-like supramolecular adducts, which have been proposed as a molecular basis of 'memory of water'.

Method for improving x-ray diffraction determinations of residual stress in nickel-base alloys

DOEpatents

Berman, R.M.; Cohen, I.

1988-04-26

A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys is discussed. Part of a predetermined area of the surface of a nickel-base alloy is covered with a dispersion. This exposes the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose, since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample. 2 figs.

Experimental determination of growth rate effect on U 6+ and Mg 2+ partitioning between aragonite and fluid at elevated U 6+ concentration

NASA Astrophysics Data System (ADS)

Gabitov, R. I.; Gaetani, G. A.; Watson, E. B.; Cohen, A. L.; Ehrlich, H. L.

2008-08-01

Results are reported from an experimental study in which the partitioning of U and Mg between aragonite and an aqueous solution were determined as a function of crystal growth rate. Crystals, identified as aragonite by X-ray diffractometry and micro-Raman spectroscopy, were grown by diffusion of CO 2 from an ammonium carbonate source into a calcium-bearing solution at temperatures of 22 and 53 °C. Hemispherical bundles (spherulites) of aragonite crystals were produced, the growth rates of which decreased monotonically from the spherulite interiors to the edges and thus provide the opportunity to examine the influence of growth rate on crystal composition. Element concentration ratios were measured using electron microprobe (EMP) and fluid composition was determined by inductively coupled plasma-mass spectrometry (ICP-MS) and atomic absorption (AA). Growth rates were determined directly by addition of a Dy spike to the fluid during the experiment that was subsequently located in an experimentally precipitated spherulite using secondary ion mass spectrometry (SIMS). At 22 °C both U/Ca and Mg/Ca partition coefficients exhibited a strong growth rate dependence when crystal growth rates were low, and became independent of growth rate when crystal growth rates were high. The U/Ca ratios in aragonite increase between 22 and 53 °C; in contrast Mg/Ca ratios show inverse dependence on temperature.

Modification of solid-state property of sulfasalazine by using the supercritical antisolvent process

NASA Astrophysics Data System (ADS)

Wu, Wei-Yi; Su, Chie-Shaan

2017-02-01

In this study, the supercritical antisolvent (SAS) process was used to recrystallize an active pharmaceutical ingredient, sulfasalazine, to modify the solid-state properties including particle size, crystal habit and polymorphic form. Supercritical CO2 and tetrahydrofuran were used as the antisolvent and solvent, respectively. SAS results obtained from different operating temperatures (35, 45, 55 and 65 °C) were compared and discussed. The results indicate that at 55 °C, spherical sulfasalazine crystals were produced and that their mean particle size was micronized to approximately 1 μm. In addition, according to the analytical results of powder X-ray diffractometry (PXRD), a novel polymorphic form of sulfasalazine was obtained after SAS. Furthermore, the spectroscopic and thermal behavior of produced sulfasalazine crystals were also studied by Fourier transform infrared spectrometry (FTIR), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Finally, SAS results obtained from different operating temperature was discussed on the basis of the mixture critical point (MCP) of CO2 and tetrahydrofuran. Operation at slightly higher than the MCP is favorable for recrystallization of sulfasalazine through SAS. These results demonstrate that the SAS process is an efficient tool for controlling and modifying the solid-state property of sulfasalazine.

Mono-Schiff-base or di-Schiff-base? Synthesis, spectroscopic, X-ray structural and DFT study of a series of Schiff-bases derived from benzil dihydrazone

NASA Astrophysics Data System (ADS)

Tan, Xue-Jie; Hao, Xiu-Qi; Zhao, Qing-Zhe; Cheng, Shuang-Shuang; Xie, Wen-Long; Xing, Dian-Xiang; Liu, Yun; Song, Lai-Zhou

2015-11-01

A series of mono- and di-Schiff-bases based on Benzil Dihydrazone (BDH) were designed and synthesized to be set as the model compounds to explain which one should be the advanced product and which parameters will determine the end-product. As the first step of a series of investigations, this article presents the syntheses and characterization of five new Schiff-bases plus one preliminary reported Schiff-base, all derived from BDH. The compounds were characterized by single crystal (or conventional powder) X-ray diffractometry, elemental analysis, m.p., 1H NMR, 13C NMR, IR and UV-Vis. Structural features of the five new Schiff-bases are similar. For instance, all molecules are nonsymmetrical/symmetrical double helix with the torsion angle of two "half-parts" about 72-97°. The Ph-Cdbnd N-Ndbnd C-Ph moiety all exists in planar and anti form, indicating significant conjugation. The crystal structures appear to be stabilized by π-stacking between the aromatic rings, as well as by intermolecular hydrogen bonds and C-H … π stacking interactions. DFT calculations have been performed to explain the trend of the experimentally measured reaction yields. In the case of the studied systems by us, the type of Schiff-bases exhibits a clear dependence on the molar ratio of reactants if the products have similar stabilities. Otherwise the importance of reaction conditions will be weakened and the most stable product will be favored.

Synthesis of core–shell structured FAU/SBA-15 composite molecular sieves and their performance in catalytic cracking of polystyrene

PubMed Central

Du, Jinlong; Shi, Chunwei; Wu, Wenyuan; Bian, Xue; Chen, Ping; Cui, Qingzhu; Cui, Zhixuan

2017-01-01

Abstract Composite molecular sieves, FAU/SBA-15, having core-shell structure were synthesized. The synthesized composite sieves were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), pyrolysis fourier transform infrared (Py-FTIR) spectroscopy, temperature programmed desorption spectra (NH3-TPD), UV Raman spectroscopy, nuclear magnetic resonance (NMR) and other techniques. XRD, SEM, TEM, N2 adsorption-desorption, mass spectrometry, NMR and EDS results showed that the composite molecular sieve contained two pore channels. Py-FTIR results showed that the addition of HY molecular sieves improved the acidity of the composite zeolite. The crystallization mechanism during the growth of FAU/SBA-15 shell was deduced from the influence of crystallization time on the synthesis of FAU/SBA-15 core-shell structured composite molecular sieve. HY dissociated partially in H2SO4 solution, and consisted of secondary structural units. This framework structure was more stable than its presence in the isolated form on the same ring or in the absence of Al. Thus it played a guiding role and connected with SBA-15 closely through the Si-O bond. This resulted in the gradual covering of the exterior surface of FAU phase by SBA-15 molecular sieves. The presence of SBA-15 restricted the formation of the other high mass components and increased the selectivity towards ethylbenzene. PMID:29383044

Strength Characteristics of Resorbable Osteoconductive Ceramics Based on Diphosphates of Calcium and Alkali Metals

NASA Astrophysics Data System (ADS)

Putlayev, V. I.; Evdokimov, P. V.; Garshev, A. V.; Prosvirin, D. V.; Klimashina, E. S.; Safronova, T. V.; Ivanov, V. K.

2014-02-01

An investigation into the strength characteristics of ceramics based on diphosphates Ca(3- x)М2 x (PO4)2 ( x = 0-1 and М = Na, K) provides evidence of composition strengthening in the range х = 0.6-0.8 containing the greatest amount of the supercooled high-temperature modification α-СаМРО4. The method of high-temperature x-ray diffractometry is used to examine thermal expansion of rhenanite phases of СаМРО4.

Anomalous magnetoelastic behaviour near morphotropic phase boundary in ferromagnetic Tb 1-xNd xCo 2 system

DOE PAGES

Murtaza, Adil; Yang, Sen; Zhou, Chao; ...

2016-08-04

In this study, we report a morphotropic phase boundary (MPB) involved ferromagnetic system Tb 1-xNd xCo 2 and reveal the corresponding structural and magnetoelastic properties of this system. With high resolution synchrotron X-ray diffractometry, the crystal structure of the TbCo 2-rich side is detected to be rhombohedral and that of NdCo 2-rich side is tetragonal below their respective Curie temperatures TC. The MPB composition Tb 0.35Nd 0.65Co 2 corresponds to the coexistence of the rhombohedral phase (R-phase) and tetragonal phase ( T-phase). Contrary to previously reported MPB involved ferromagnetic systems, the MPB composition of Tb 0.35Nd 0.65Co 2 shows minimummore » magnetization which can be understood as compensation of sublattice moments between the R-phase and the T-phase. Furthermore, magnetostriction of Tb 1-xNd xCo 2 decreases with increasing Nd concentration until x = 0.8 and then increases in the negative direction with further increasing Nd concentration; the optimum point for magnetoelastic properties lies towards the rhombohedral phase. Finally, our work not only shows an anomalous type of ferromagnetic MPB but also provides an effective way to design functional materials.« less

Direct observation of the ferroelectric polarization in the layered perovskite Bi{sub 4}Ti{sub 3}O{sub 12}

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

Urushihara, Daisuke; Asaka, Toru, E-mail: asaka.toru@nitech.ac.jp; Frontier Research Institute for Materials Science, Nagoya Institute of Technology, Nagoya 466-8555

We investigated the crystal structure and ferroelectric domains of Bi{sub 4}Ti{sub 3}O{sub 12} (BTO) by means of transmission electron microscopy (TEM) and single-crystal X-ray diffractometry. From the extinction rule, we determined that the space group in the ferroelectric phase of BTO is P1a1 rather than B2cb and B1a1 which have been proposed previously. We successfully refined the crystal structure based on the space group P1a1. The 180° and 90° ferroelectric domain structures were observed by the [001]-zone dark-field TEM imaging. In the 180° domain structure, we determined that one component of the polarization vector is parallel to the a-axis. Anmore » annular bright-field scanning transmission electron microscopy (ABF-STEM) was performed for the direct observation of the crystal structures. The ABF-STEM images displayed the contrasts with respect to every atomic position in spite of the highly distorted structure of BTO. We could evaluate the tilting and distortion of the [TiO{sub 6}] octahedra relatively. Therefore, we directly observed the ferroelectric displacements of Bi and Ti ions.« less

Solid-state characterization of mefenamic acid.

PubMed

Panchagnula, Ramesh; Sundaramurthy, Prakash; Pillai, Omathanu; Agrawal, Shrutidevi; Raj, Yasvanth Ashok

2004-04-01

The purpose of this study was to characterize mefenamic acid (MA) from commercial samples and samples crystallized from different solvents. Various techniques used for characterization included microscopy (hot stage microscopy, scanning electron microscopy), intrinsic dissolution rate, differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) spectroscopy and powder X-ray diffractometry (pXRD). The commercial samples varied in their crystal habit, thermal behavior, and intrinsic dissolution rate. It was found that the commercial samples were polymorphic Form I, which converted to Form II on heating in a DSC pan. Similarly, compression in an intrinsic dissolution rate (IDR) press resulted in the conversion of Form I to Form II. On the other hand, the samples recrystallized from different solvents under varying conditions yielded different crystal habits. Stirring and degree of supersaturation significantly influenced the crystal habit in all the solvents used in the study. Samples crystallized from ethanol and tetrahydrofuran yielded Form I, which behaved similarly to the commercial samples (M1 and M3). Recrystallization from ethyl acetate at a fast cooling rate yielded Form I, which on melting crystallized to Form II. The form I crystallized from ethyl acetate by fast cooling converted partially to form II on storing at ambient conditions. Forms I and II of MA were enantiotropically related. The results demonstrate the variable material characteristics of the commercial samples of MA and the influence of the crystallizing conditions on the formation of the polymorphs. Copyright 2004 Wiley-Liss, Inc. and the American Pharmacists Association.

Site specific mineral composition and microstructure of human supra-gingival dental calculus.

PubMed

Hayashizaki, Junko; Ban, Seiji; Nakagaki, Haruo; Okumura, Akihiko; Yoshii, Saori; Robinson, Colin

2008-02-01

Dental calculus has been implicated in the aetiology of several periodontal conditions. Its prevention and removal are therefore desirable clinical goals. While it is known that calculus is very variable in chemical composition, crystallinity and crystallite size little is known about site specific variability within a dentition and between individuals. With this in mind, a study was undertaken to investigate the comparative site specific nature and composition of human dental supra-gingival dental calculus obtained from 66 male patients visiting for their dental check-up using fluorescent X-ray spectroscopy, X-ray diffractometry and Fourier transform infrared spectroscopy. The supra-gingival dental calculus formed on the lingual surfaces of lower anterior teeth and the buccal surfaces of upper molar teeth were classified into four types based on calcium phosphate phases present. There was significant difference in composition of the crystal phase types between lower and upper teeth (p<0.01). There was no significant difference in crystal size between dental calculus on anterior or molar teeth of all samples. The degree of crystallinity of dental calculus formed on the upper molar teeth was higher than that formed on the lower anterior teeth (p<0.01). The CO(3)(2-) contents in dental calculus formed on the lower anterior teeth were higher than on upper molar teeth (p<0.05) which might explain the difference in crystallinity. Magnesium and Si contents and Ca:P ratio on the other hand showed no significant difference between lower and upper teeth. It was concluded that the crystal phases, crystallinity and CO(3)(2-) contents of human dental supra-gingival dental calculus is related to its location in the mouth.

Nacre-like calcium carbonate controlled by ionic liquid/graphene oxide composite template.

PubMed

Yao, Chengli; Xie, Anjian; Shen, Yuhua; Zhu, Jinmiao; Li, Hongying

2015-06-01

Nacre-like calcium carbonate nanostructures have been mediated by an ionic liquid (IL)-graphene oxide (GO) composite template. The resultant crystals were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, and X-ray powder diffractometry (XRD). The results showed that either 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]BF4) or graphene oxide can act as a soft template for calcium carbonate formation with unusual morphologies. Based on the time-dependent morphology changes of calcium carbonate particles, it is concluded that nacre-like calcium carbonate nanostructures can be formed gradually utilizing [BMIM]BF4/GO composite template. During the process of calcium carbonate formation, [BMIM]BF4 acted not only as solvents but also as morphology templates for the fabrication of calcium carbonate materials with nacre-like morphology. Based on the observations, the possible mechanisms were also discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Fabrication of Ti-0.48Al Alloy by Centrifugal Casting.

PubMed

Park, Jong Bum; Lee, Jung-Il; Ryu, Jeong Ho

2018-09-01

Many of the unique properties of TiAl alloys that make are attractive for use in high-temperature structural applications also make it challenging to process them into useful products. Cast TiAl is rapidly nearing commercialization, particularly in the vehicle industry, owing to its low production cost. In this study, the centrifugal casting of a TiAl (Ti-48%Al, mole fraction) turbocharger was simulated and an experimental casting was created in vacuum using an induction melting furnace coupled to a ceramic composite mold. Numerical simulation results agreed with the experiment. The crystal structure, microstructure, and chemical composition of the TiAl prepared by centrifugal casting were studied by X-ray diffractometry, optical microscopy, field emission scanning electron microscopy (FE-SEM) and energy dispersive spectroscopy (EDS). FE-SEM and EDS examinations of the TiAl casting revealed that the thickness of the oxide layer (α-case) was typically less than 35 μm.

Experimental and calculated structural parameters of 5-trihalomethyl-4,5-dihydro-1 H-pyrazole derivatives, novel analgesic agents

NASA Astrophysics Data System (ADS)

Machado, Pablo; Campos, Patrick T.; Lima, Glauber R.; Rosa, Fernanda A.; Flores, Alex F. C.; Bonacorso, Helio G.; Zanatta, Nilo; Martins, Marcos A. P.

2009-01-01

The crystal structures of four novel analgesic agents, methyl 5-hydroxy-3- or 4-methyl-5-trichloro[trifluoro]methyl-4,5-dihydro-1 H-pyrazole-1-carboxylate, have been determined by X-ray diffractometry. The data demonstrated that the molecular packing was stabilized mainly by O sbnd H⋯O hydrogen bonds of the 5-hydroxy and 1-carboxymethyl groups. The 4,5-dihydro-1 H-pyrazole rings were obtained as almost planar structures showing RMS deviation at a range of 0.0052-0.0805 Å. Additionally, computational investigation using semi-empirical AM1 and PM3 methods were performed to find a correlation between experimental and calculated geometrical parameters. The data obtained suggest that the structural data furnished by the AM1 method is in better agreement with those experimentally determined for the above compounds.

Crystallization of D-mannitol in binary mixtures with NaCl: phase diagram and polymorphism.

PubMed

Telang, Chitra; Suryanarayanan, Raj; Yu, Lian

2003-12-01

To study the crystallization, polymorphism, and phase behavior of D-mannitol in binary mixtures with NaCl to better understand their interactions in frozen aqueous solutions. Differential scanning calorimetry, hot-stage microscopy, Raman microscopy, and variable-temperature X-ray diffractometry were used to characterize D-mannitol-NaCl mixtures. NaCl and D-mannitol exhibited significant melt miscibility (up to 7.5% w/w or 0.20 mole fraction of NaCl) and a eutectic phase diagram (eutectic composition 7.5% w/w NaCl; eutectic temperature 150 degrees C for the alpha and beta polymorphs of D-mannitol and 139 degrees C for the delta). The presence of NaCl did not prevent mannitol from crystallizing but, depending on sample size, affected the polymorph crystallized: below 10 mg, delta was obtained; above 100 mg, alpha was obtained. Pure mannitol crystallized under the same conditions first as the delta polymorph and then as the a polymorph, with the latter nucleating on the former. KCl showed similar eutectic points and melt miscibility with D-mannitol as NaCl. LiCl yielded lower eutectic melting points, inhibited the crystallization of D-mannitol during cooling, and enabled the observation of its glass transition. Despite their structural dissimilarity, significant melt miscibility exists between D-mannitol and NaCl. Their phase diagram has been determined and features polymorph-dependent eutectic points. NaCl influences the polymorphic behavior of mannitol, and the effect is linked to the crystallization of mannitol in two polymorphic stages.

A photoluminescence, thermoluminescence and electron paramagnetic resonance study of EFG grown europium doped lithium fluoride (LiF) crystals

NASA Astrophysics Data System (ADS)

Seth, Pooja; Swati, G.; Haranath, D.; Rao, S. M. D.; Aggarwal, Shruti

2018-07-01

Europium (Eu) doped LiF crystals have been grown by the Edge-defined film fed growth (EFG) technique. The designing and installation of the furnace used for the growth of the crystals have been discussed in detail. In the present study, Eu (Eu2O3) has been doped in LiF in different concentration (0.02-0.2 wt %). X-ray diffractometry (XRD) and Energy Dispersive X-ray (EDX) spectroscopy confirms the incorporation of Eu in LiF. The influence of Eu on LiF has been investigated through photoluminescence (PL), thermoluminescence (TL) and electron paramagnetic resonance (EPR) in as-grown and annealed crystals. PL emission spectra shows the presence of both Eu3+ and Eu2+ form in the as-grown crystals which is confirmed by EPR results. Whereas, in annealed crystals, Eu is present predominantly as Eu2+ form. This suggests that growing crystals at high temperature (∼900 °C) in argon gas atmosphere through EFG technique favours the reduction of Eu3+ → Eu2+. This reduction phenomenon has been explained on the basis of charge compensation model. TL study of the LiF: Eu (0.02-0.2 wt %) crystals has been done after irradiation with Co60 gamma rays. In this study, it has been observed that the TL intensity as well as glow curve structure of LiF: Eu crystals are a strong function of Eu concentration. The maximum TL is observed at Eu concentration of 0.05 wt% at which a well defined glow curve structure with a prominent peak at 185 °C and a small peak at 253 °C. Beyond this concentration (0.05 wt %), TL intensity decreases due to aggregation of defects in the host. The peak at 185 °C in LiF: Eu (0.05 wt %) is certainly due to the presence of Eu2+ associated defects which is also supported by the PL spectra. It has been observed that Eu doping have a key role in creation of more defect levels which lead to the increased number of electron and hole traps. Further, trapping parameters are analysed using glow curve deconvolution method to have an insight study of TL phenomena. Further, TL glow curve structure of as-grown and annealed crystal are distinct which may be attributed to the nature of defect traps formed inside the LiF.

Pseudomorphic GeSiSn, SiSn and Ge layers in strained heterostructures

NASA Astrophysics Data System (ADS)

Timofeev, V. A.; Nikiforov, A. I.; Tuktamyshev, A. R.; Mashanov, V. I.; Loshkarev, I. D.; Bloshkin, A. A.; Gutakovskii, A. K.

2018-04-01

The GeSiSn, SiSn layer growth mechanisms on Si(100) were investigated and the kinetic diagrams of the morphological GeSiSn, SiSn film states in the temperature range of 150 °C-450 °C at the tin content from 0% to 35% were built. The phase diagram of the superstructural change on the surface of Sn grown on Si(100) in the annealing temperature range of 0 °C-850 °C was established. The specular beam oscillations were first obtained during the SiSn film growth from 150 °C to 300 °C at the Sn content up to 35%. The transmission electron microscopy and x-ray diffractometry data confirm the crystal perfection and the pseudomorphic GeSiSn, SiSn film state, and also the presence of smooth heterointerfaces between GeSiSn or SiSn and Si. The photoluminescence for the multilayer periodic GeSiSn/Si structures in the range of 0.6-0.8 eV was detected. The blue shift with the excitation power increase is observed suggesting the presence of a type II heterostructure. The creation of tensile strained Ge films, which are pseudomorphic to the underlying GeSn layer, is confirmed by the results of the formation and analysis of the reciprocal space map in the x-ray diffractometry. The tensile strain in the Ge films reached the value in the range of 0.86%-1.5%. The GeSn buffer layer growth in the Sn content range from 8% to 12% was studied. The band structure of heterosystems based on pseudomorphic GeSiSn, SiSn and Ge layers was calculated and the valence and conduction band subband position dependences on the Sn content were built. Based on the calculation, the Sn content range in the GeSiSn, SiSn, and GeSn layers, which corresponds to the direct bandgap GeSiSn, SiSn, and Ge material, was obtained.

Use of glancing angle X-ray powder diffractometry to depth-profile phase transformations during dissolution of indomethacin and theophylline tablets.

PubMed

Debnath, Smita; Predecki, Paul; Suryanarayanan, Raj

2004-01-01

The purpose of this study was (i) to develop glancing angle x-ray powder diffractometry (XRD) as a method for profiling phase transformations as a function of tablet depth; and (ii) to apply this technique to (a) study indomethacin crystallization during dissolution of partially amorphous indomethacin tablets and to (b) profile anhydrate --> hydrate transformations during dissolution of theophylline tablets. The intrinsic dissolution rates of indomethacin and theophylline were determined after different pharmaceutical processing steps. Phase transformations during dissolution were evaluated by various techniques. Transformation in the bulk and on the tablet surface was characterized by conventional XRD and scanning electron microscopy, respectively. Glancing angle XRD enabled us to profile these transformations as a function of depth from the tablet surface. Pharmaceutical processing resulted in a decrease in crystallinity of both indomethacin and theophylline. When placed in contact with the dissolution medium, while indomethacin recrystallized, theophylline anhydrate rapidly converted to theophylline monohydrate. Due to intimate contact with the dissolution medium, drug transformation occurred to a greater extent at or near the tablet surface. Glancing angle XRD enabled us to depth profile the extent of phase transformations as a function of the distance from the tablet surface. The processed sample (both indomethacin and theophylline) transformed more rapidly than did the corresponding unprocessed drug. Several challenges associated with the glancing angle technique, that is, the effects of sorbed water, phase transformations during the experimental timescale, and the influence of phase transformation on penetration depth, were addressed. Increased solubility, and consequently dissolution rate, is one of the potential advantages of metastable phases. This advantage is negated if, during dissolution, the metastable to stable transformation rate > dissolution rate. Glancing angle XRD enabled us to quantify and thereby profile phase transformations as a function of compact depth. The technique has potential utility in monitoring surface reactions, both chemical decomposition and physical transformations, in pharmaceutical systems.

Evolution of Constitution, Structure, and Morphology in FeCo-Based Multicomponent Alloys

NASA Astrophysics Data System (ADS)

Li, R.; Stoica, M.; Liu, G.; Eckert, J.

2010-07-01

Constituent phases, melting behaviors, and microstructure of multicomponent (Fe0.5Co0.5) x (Mo0.1C0.2B0.5Si0.2)100- x alloys ( x = 95, 90, 85, 80, and 70) produced by copper mold casting were evaluated by various analysis techniques, i.e., X-ray diffractometry, scanning electronic microscopy with energy dispersive X-ray spectrometry, and differential scanning calorimetry. Metastable Fe3C- and Cr23C6-type phases were identified in the chill-cast alloys. A schematic illustration was proposed to explain the evolution of constituent phases and microstructure for the alloys with x = 95, 90, and 85 during the solidification process, which could be applicable to controlling microstructural formation of other multicomponent alloys with similar microstructures by artificially adjusting the composition.

Crystals for krypton helium-alpha line emission microscopy

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

Koch, Jeffrey A.; Haugh, Michael J.

2018-04-17

A system for reflecting and recording x-ray radiation from an x-ray emitting event to characterize the event. A crystal is aligned to receive radiation along a first path from an x-ray emitting event. Upon striking the crystal, the x-ray reflects from the crystal along a second path due to a reflection plane of the crystal defined by one of the following Miller indices: (9,7,3) or (11,3,3). Exemplary crystalline material is germanium. The x-rays are reflected to a detector aligned to receive reflected x-rays that are reflected from the crystal along the second path and the detector generates a detector signalmore » in response to x-rays impacting the detector. The detector may include a CCD electronic detector, film plates, or any other detector type. A processor receives and processes the detector signal to generate reflection data representing the x-rays emitted from the x-ray emitting event.« less

Four new polymorphic forms of suplatast tosilate.

PubMed

Nagai, Keiko; Ushio, Takanori; Miura, Hidenori; Nakamura, Takashi; Moribe, Kunikazu; Yamamoto, Keiji

2014-01-02

We found four new polymorphic forms (γ-, ε-, ζ-, and η-forms) of suplatast tosilate (ST) by recrystallization and seeding with ST-analogous compounds; three polymorphic forms (α-, β-, and δ-forms) of ST have been previously reported. The physicochemical properties of these new forms were investigated using infrared (IR) spectroscopy, solid-state nuclear magnetic resonance (NMR) spectroscopy, differential scanning calorimetry, and powder X-ray diffractometry. The presence of hydrogen bonds in the new forms was assessed from the IR and solid-state NMR spectra. The crystal structures of the ε- and η-forms were determined from their powder X-ray diffraction data using the direct space approach and the Monte Carlo method, followed by Rietveld refinement. The structures determined for the ε- and η-forms supported the presence of hydrogen bonds between the ST molecules, as the IR and solid-state NMR spectra indicated. The thermodynamic characteristics of the seven polymorphic forms were evaluated by determining the solubility of each form. The α-form was the most insoluble in 2-propanol at 35°C, and was thus concluded to be the most stable form. The ε-form was the most soluble, and a polymorphic transition from the ε- to the α-form was observed during solubility testing. Copyright © 2013 Elsevier B.V. All rights reserved.

Passivation of hematite nanorod photoanodes with a phosphorus overlayer for enhanced photoelectrochemical water oxidation

NASA Astrophysics Data System (ADS)

Xiong, Dehua; Li, Wei; Wang, Xiaoguang; Liu, Lifeng

2016-09-01

Hematite (i.e., α-Fe2O3) nanorod photoanodes passivated with a phosphorus overlayer have been fabricated by decomposing sodium hypophosphite (NaH2PO2) at a low temperature over the hematite nanorod surface. Extensive scanning electron microscopy, transmission electron microscopy, x-ray diffractometry and UV-vis spectroscopy characterizations confirm that conformal deposition of an amorphous phosphorus overlayer does not change the crystal structure, morphology, and optical absorption properties of hematite photoanodes. X-ray photoelectron spectroscopy reveals that phosphorus in the deposited overlayer exists in an oxidized state. Comprehensive steady-state polarization, transient photocurrent response, and impedance spectroscopy measurements as well as Mott-Schottky analysis manifest that the phosphorus overlayer is able to effectively passivate surface states and suppress electron-hole recombination, substantially enhancing the photocurrent for water oxidation. Combining the phosphorization treatment with two-step thermal activation, a photocurrent density of 1.1 mA cm-2 is achieved at 1.23 V versus reversible hydrogen electrode under illumination of 100 mW cm-2, ca 55 times higher than that of the non-activated pristine hematite photoanode measured under the same conditions. The simple and fast phosphorization strategy we present here can be readily applied to passivate surfaces of other semiconductor photoelectrodes to improve their photoelectrochemical performance.

The effect of X-ray exposure on Ba2SiO4:Eu3+

NASA Astrophysics Data System (ADS)

Volhard, Max-Fabian; Jüstel, Thomas

2018-03-01

The ortho-silicates Ba2SiO4:Eu3+ and Ba2SiO4:Eu2+ are well-established materials for fluorescent light sources, e.g., phosphor converted LEDs. Samples containing Eu2+or Eu3+were synthesised by the solid-state-method, and the phase purity was determined by X-ray powder diffractometry. The photoluminescence of both phosphors was examined as a function of the pre-treatment. Upon irradiation of Ba2SiO4:Eu3+ with X-rays (tungsten target source), the reduction of Eu3+ towards Eu2+ was observed. This reduction behaviour was thoroughly recorded, and the linearity of the process was determined. Furthermore, the relationship between the acceleration voltage and the reduction process is discussed.

Interactions between carbamazepine and polyethylene glycol (PEG) 6000: characterisations of the physical, solid dispersed and eutectic mixtures.

PubMed

Naima, Z; Siro, T; Juan-Manuel, G D; Chantal, C; René, C; Jerome, D

2001-02-01

The influence of a hydrophilic carrier (PEG 6000) on the polymorphism of carbamazepine, an antiepileptic drug, was investigated in binary physical mixtures and solid dispersions by means of differential scanning calorimetry (DSC), thermal gravimetry, hot-stage microscopy (HSM), and X-ray diffractometry, respectively. This study provides also an attempt to develop a method to calculate more precisely the eutectic composition. In rather ideal physical mixtures, carbamazepine was found as monoclinic Form III. In solid dispersions, the drug was found to crystallize as trigonal Form II; a eutectic invariant in the PEG 6000-rich composition domain (6% of carbamazepine mass) was evidenced by DSC experiments and confirmed by HSM observations. In the binary phase diagram the ideal carbamazepine liquidus curve was located at temperatures higher than the respective experimental ones. This suggests that drug can be maintained in the liquid state in the temperature-mass fraction (T--x) region between the two carbamazepine liquidus curves. This indicates in turn that attractive interactions occur between carbamazepine and PEG 6000-chains. These interactions have been also claimed to prevent carbamazepine from degradation into iminostilbene (a compound resulting from the chemical degradation of carbamazepine which is postulated to be responsible for the idiosyncratic toxicity of the drug) and thought to lead to the crystallization of metastable Carbamazepine II from melt. The negative excess entropy for eutectic mixtures indicated that the drug crystals are finely dispersed in the bulk of polymer chains.

Precision mechanical structure of an ultra-high-resolution spectrometer for inelastic X-ray scattering instrument

DOEpatents

Shu, Deming; Shvydko, Yuri; Stoupin, Stanislav A.; Khachatryan, Ruben; Goetze, Kurt A.; Roberts, Timothy

2015-04-14

A method and an ultrahigh-resolution spectrometer including a precision mechanical structure for positioning inelastic X-ray scattering optics are provided. The spectrometer includes an X-ray monochromator and an X-ray analyzer, each including X-ray optics of a collimating (C) crystal, a pair of dispersing (D) element crystals, anomalous transmission filter (F) and a wavelength (W) selector crystal. A respective precision mechanical structure is provided with the X-ray monochromator and the X-ray analyzer. The precision mechanical structure includes a base plate, such as an aluminum base plate; positioning stages for D-crystal alignment; positioning stages with an incline sensor for C/F/W-crystal alignment, and the positioning stages including flexure-based high-stiffness structure.

Lysozyme Crystal

NASA Technical Reports Server (NTRS)

2004-01-01

To the crystallographer, this may not be a diamond but it is just as priceless. A Lysozyme crystal grown in orbit looks great under a microscope, but the real test is X-ray crystallography. The colors are caused by polarizing filters. Proteins can form crystals generated by rows and columns of molecules that form up like soldiers on a parade ground. Shining X-rays through a crystal will produce a pattern of dots that can be decoded to reveal the arrangement of the atoms in the molecules making up the crystal. Like the troops in formation, uniformity and order are everything in X-ray crystallography. X-rays have much shorter wavelengths than visible light, so the best looking crystals under the microscope won't necessarily pass muster under the X-rays. In order to have crystals to use for X-ray diffraction studies, crystals need to be fairly large and well ordered. Scientists also need lots of crystals since exposure to air, the process of X-raying them, and other factors destroy them. Growing protein crystals in space has yielded striking results. Lysozyme's structure is well known and it has become a standard in many crystallization studies on Earth and in space.

Devitrification studies of wollastonite-tricalcium phosphate eutectic glass.

PubMed

Magallanes-Perdomo, M; Pena, P; De Aza, P N; Carrodeguas, R G; Rodríguez, M A; Turrillas, X; De Aza, S; De Aza, A H

2009-10-01

The present paper describes and discusses the devitrification and crystallization process of wollastonite-tricalcium phosphate (W-TCP) eutectic glass. This process was studied in situ from room temperature up to 1375 degrees C, by neutron diffractometry in vacuum. The data obtained were combined and compared with those performed in ambient atmosphere by differential thermal analysis and with those of samples fired in air at selected temperatures, and then cooled down and subsequently studied by laboratory XRD and field emission scanning electron microscopy fitted with energy X-ray dispersive spectroscopy. The experimental evidence indicates that the devitrification of W-TCP eutectic glass begins at approximately 870 degrees C with the crystallization of a Ca-deficient apatite phase, followed by wollastonite-2M (CaSiO(3)) crystallization at approximately 1006 degrees C. At 1375 degrees C, the bio-glass-ceramic is composed of quasi-rounded colonies formed by a homogeneous mixture of pseudowollastonite (CaSiO(3)) and alpha-tricalcium phosphate (Ca(3)(PO(4))(2)). This microstructure corresponds to irregular eutectic structures. It was also found that it is possible to obtain from the eutectic composition of the wollastonite-tricalcium phosphate binary system a wide range of bio-glass-ceramics, with different crystalline phases present, through appropriate design of thermal treatments.

High-throughput cocrystal slurry screening by use of in situ Raman microscopy and multi-well plate.

PubMed

Kojima, Takashi; Tsutsumi, Shunichirou; Yamamoto, Katsuhiko; Ikeda, Yukihiro; Moriwaki, Toshiya

2010-10-31

Cocrystal has attracted much attention in order to improve poor physicochemical properties, since cocrystal former crystallize with the ionic drugs as well as nonionic drugs. Cocrystal screening was usually conducted by crystallization, slurry and co-grinding techniques, however sensitivity, cost and time for screening were limited because of issues such as dissociation of cocrystal during crystallization and cost and time required for slurry and co-grinding methods. To overcome these issues, novel high-throughput cocrystal slurry screening was developed by using in situ Raman microscope and a multi-well plate. Cocrystal screening of indomethacin was conducted with 46 cocrystal formers and potential cocrystals were prepared on a large scale for the characterization with powder X-ray diffractometry, thermal analysis, and Raman microscopy and (1)H NMR spectroscopy. Compared with the characterization of scale-up cocrystals, the cocrystal screening indicated that indomethacin structured novel cocrystals with D/L-mandelic acid, nicotinamide, lactamide and benzamide which was not obtained in the screening with crystallization technique previously reported. In addition, the screening provided not only information of cocrystal formation within a day but also information of equilibrium of cocrystal formation and polymorphic transformation in one screening. Information obtained in this screening allows effective solid form selection by saving cost and time for the development. Copyright © 2010 Elsevier B.V. All rights reserved.

Curved focusing crystals for hard X-ray astronomy

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

Ferrari, C., E-mail: ferrari@imem.cnr.it; Buffagni, E.; Bonnini, E.

A lens made by a properly arranged array of crystals can be used to focus x-rays of energy ranging from 30 to 500 keV for x-ray astronomy. Mosaic or curved crystals can be employed as x-ray optical elements. In this work self standing curved focusing Si and GaAs crystals in which the lattice bending is induced by a controlled damaging process on one side of planar crystals are characterized. Diffraction profiles in Laue geometry have been measured in crystals at x-ray energies E = 17, 59 and 120 keV. An enhancement of diffraction efficiency is found in asymmetric geometries.

Direct detection of x-rays for protein crystallography employing a thick, large area CCD

DOEpatents

Atac, Muzaffer; McKay, Timothy

1999-01-01

An apparatus and method for directly determining the crystalline structure of a protein crystal. The crystal is irradiated by a finely collimated x-ray beam. The interaction of the x-ray beam with the crystal produces scattered x-rays. These scattered x-rays are detected by means of a large area, thick CCD which is capable of measuring a significant number of scattered x-rays which impact its surface. The CCD is capable of detecting the position of impact of the scattered x-ray on the surface of the CCD and the quantity of scattered x-rays which impact the same cell or pixel. This data is then processed in real-time and the processed data is outputted to produce a image of the structure of the crystal. If this crystal is a protein the molecular structure of the protein can be determined from the data received.

Projection x-ray topography system at 1-BM x-ray optics test beamline at the advanced photon source

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

Stoupin, Stanislav, E-mail: sstoupin@aps.anl.gov; Liu, Zunping; Trakhtenberg, Emil

2016-07-27

Projection X-ray topography of single crystals is a classic technique for the evaluation of intrinsic crystal quality of large crystals. In this technique a crystal sample and an area detector (e.g., X-ray film) collecting intensity of a chosen crystallographic reflection are translated simultaneously across an X-ray beam collimated in the diffraction scattering plane (e.g., [1, 2]). A bending magnet beamline of a third-generation synchrotron source delivering x-ray beam with a large horizontal divergence, and therefore, a large horizontal beam size at a crystal sample position offers an opportunity to obtain X-ray topographs of large crystalline samples (e.g., 6-inch wafers) inmore » just a few exposures. Here we report projection X-ray topography system implemented recently at 1-BM beamline of the Advanced Photon Source. A selected X-ray topograph of a 6-inch wafer of 4H-SiC illustrates capabilities and limitations of the technique.« less

Microgravity

NASA Image and Video Library

2004-04-15

To the crystallographer, this may not be a diamond but it is just as priceless. A Lysozyme crystal grown in orbit looks great under a microscope, but the real test is X-ray crystallography. The colors are caused by polarizing filters. Proteins can form crystals generated by rows and columns of molecules that form up like soldiers on a parade ground. Shining X-rays through a crystal will produce a pattern of dots that can be decoded to reveal the arrangement of the atoms in the molecules making up the crystal. Like the troops in formation, uniformity and order are everything in X-ray crystallography. X-rays have much shorter wavelengths than visible light, so the best looking crystals under the microscope won't necessarily pass muster under the X-rays. In order to have crystals to use for X-ray diffraction studies, crystals need to be fairly large and well ordered. Scientists also need lots of crystals since exposure to air, the process of X-raying them, and other factors destroy them. Growing protein crystals in space has yielded striking results. Lysozyme's structure is well known and it has become a standard in many crystallization studies on Earth and in space.

Heats of immersion of titania powders in primer solutions

NASA Technical Reports Server (NTRS)

Siriwardane, R.; Wightman, J. P.

1983-01-01

The oxide layer present on titanium alloys can play an important role in determining the strength and durability of adhesive bonds. Here, three titania powders in different crystalline phases, rutile-R1, anatase-A1, and anatase-A2, are characterized by several techniques. These include microelectrophoresis, X-ray diffractometry, surface area pore volume analysis, X-ray photoelectron spectroscopy, and measurements of the heats of immersion. Of the three powders, R1 has the highest heat of immersion in water, while the interaction between water and A1 powder is low. Experimental data also suggest a specific preferential interaction of polyphenylquinoxaline with anatase.

Anomalous magnetoelastic behaviour near morphotropic phase boundary in ferromagnetic Tb{sub 1-x}Nd{sub x}Co{sub 2} system

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

Murtaza, Adil; Yang, Sen, E-mail: yang.sen@mail.xjtu.edu.cn; Zhou, Chao

2016-08-01

In this work, we report a morphotropic phase boundary (MPB) involved ferromagnetic system Tb{sub 1-x}Nd{sub x}Co{sub 2} and reveal the corresponding structural and magnetoelastic properties of this system. With high resolution synchrotron X-ray diffractometry, the crystal structure of the TbCo{sub 2}-rich side is detected to be rhombohedral and that of NdCo{sub 2}-rich side is tetragonal below their respective Curie temperatures T{sub C}. The MPB composition Tb{sub 0.35}Nd{sub 0.65}Co{sub 2} corresponds to the coexistence of the rhombohedral phase (R-phase) and tetragonal phase (T-phase). Contrary to previously reported MPB involved ferromagnetic systems, the MPB composition of Tb{sub 0.35}Nd{sub 0.65}Co{sub 2} shows minimummore » magnetization which can be understood as compensation of sublattice moments between the R-phase and the T-phase. Furthermore, magnetostriction of Tb{sub 1-x}Nd{sub x}Co{sub 2} decreases with increasing Nd concentration until x = 0.8 and then increases in the negative direction with further increasing Nd concentration; the optimum point for magnetoelastic properties lies towards the rhombohedral phase. Our work not only shows an anomalous type of ferromagnetic MPB but also provides an effective way to design functional materials.« less

Chemical compositions, infrared spectroscopy, and X-ray diffractometry study on brown-rotted woods

Treesearch

Gai-Yun Li; Luo-Hua Huang; Chung Hse; Te-Fu Qin

2011-01-01

The effect of brown-rot decay on the chemical composition and crystallinity of Masson pine was studied by exposing it to Wolfiporia cocos (Schwein.) Ryvarden and Gilbn. for durations of up to 15 weeks in the field. The holocellulose content, α-cellulose content, and wood crystallinity decreased slowly in the initial stage, followed by a significant reduction...

Tri-functional Fe2O3-encased Ag-doped ZnO nanoframework: magnetically retrievable antimicrobial photocatalyst

NASA Astrophysics Data System (ADS)

Karunakaran, Chockalingam; Vinayagamoorthy, Pazhamalai

2016-11-01

Fe2O3-encased ZnO nanoframework was obtained by hydrothermal method and was doped with Ag through photoreduction process. Energy dispersive x-ray spectroscopy, transmission electron microscopy (TEM), high resolution TEM, selected area electron diffractometry, x-ray diffractometry and Raman spectroscopy were employed for the structural characterization of the synthesized material. While the charge transfer resistance of the prepared nanomaterial is larger than those of Fe2O3 and ZnO the coercivity of the nanocomposite is less than that of hydrothermally obtained Fe2O3 nanostructures. Although Fe2O3/Ag-ZnO exhibits weak visible light absorption its band gap energy does not differ from that of ZnO. The photoluminescence of the fabricated nanoframework is similar to that of ZnO. The radiative recombination of charge carriers is slightly slower in Fe2O3/Ag-ZnO than in ZnO. The synthesized Fe2O3-encased Ag-doped ZnO, under UV A light, exhibits sustainable photocatalytic activity to degrade dye and is magnetically recoverable. Also, the Fe2O3/Ag-ZnO nanocomposite disinfects bacteria effectively in absence of direct illumination.

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

DOEpatents

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

2001-01-01

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

Leaching behavior and ESEM characterization of water-sensitive mudstone in southwestern Taiwan.

PubMed

Chen, Hung-Ta; Lin, Tzong-Tzeng; Chang, Juu-En

2003-05-01

This investigation attempts to understand the critical soluble salts in natural mudstone and the leaching, microstructural, and microchemical characteristics in soaked mudstone using scanning electron microscopy (SEM)/energy-dispersive X-ray analysis (EDAX), X-ray fluorescence spectrometry (XRF), X-ray diffractometry (XRD), conductivity measurement, ion chromatography (IC), and environmental scanning electron microscopy (ESEM)/EDAX techniques. Natural mudstone probably includes soluble salts such as Na2SO4, NaCl, NaCO3, and CaCO3. The dissolution of Na2SO4 controls water-sensitive mudstone very susceptible to slaking and dispersion. ESEM micrographs clearly show evidence of mudstone-slaking during soaking since the visible pores are filled with small aggregative masses. A calcium-bearing precipitate from the soaked mudstone is speculated to be attributable to the decomposition of the hydrated product of the fresh mudstone.

A graphite crystal polarimeter for stellar X-ray astronomy.

NASA Technical Reports Server (NTRS)

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

1972-01-01

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

Neodymium(III) Complexes of Dialkylphosphoric and Dialkylphosphonic Acids Relevant to Liquid-Liquid Extraction Systems

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

Lumetta, Gregg J.; Sinkov, Sergey I.; Krause, Jeanette A.

2016-01-27

The complexes formed during the extraction of neodymium(III) into hydrophobic solvents containing acidic organophosphorus extractants were probed by single-crystal X-ray diffractometry, visible spectrophotometry, and Fourier-transform infrared spectroscopy. The crystal structure of the compound Nd(DMP)3 (1, DMP = dimethyl phosphate) revealed a polymeric arrangement in which each Nd(III) center is surrounded by six DMP oxygen atoms in a pseudo-octahedral environment. Adjacent Nd(III) ions are bridged by (MeO)2POO– anions, forming the polymeric network. The diffuse reflectance visible spectrum of 1 is nearly identical to that of the solid that is formed when an n-dodecane solution of di-(2-ethylhexyl)phosphoric acid (HA) is saturated withmore » Nd(III), indicating a similar coordination environment around the Nd center in the NdA3 solid. The visible spectrum of the HA solution fully loaded with Nd(III) is very similar to that of the NdA3 material, both displaying hypersensitive bands characteristic of an pseudo-octahedral coordination environment around Nd. These spectral characteristics persisted across a wide range of organic Nd concentrations, suggesting that the pseudo-octahedral coordination environment is maintained from dilute to saturated conditions.« less

Growth of ferroelectric Ba{sub 0.8}Sr{sub 0.2}TiO{sub 3} epitaxial films by ultraviolet pulsed laser irradiation of chemical solution derived precursor layers

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

Queraltó, A.; Pérez del Pino, A., E-mail: aperez@icmab.es; Mata, M. de la

2015-06-29

Highly crystalline epitaxial Ba{sub 0.8}Sr{sub 0.2}TiO{sub 3} (BST) thin-films are grown on (001)-oriented LaNiO{sub 3}-buffered LaAlO{sub 3} substrates by pulsed laser irradiation of solution derived barium-zirconium-titanium precursor layers using a UV Nd:YAG laser source at atmospheric conditions. The structural analyses of the obtained films, studied by X-ray diffractometry and transmission electron microscopy, demonstrate that laser processing allows the growth of tens of nm-thick BST epitaxial films with crystalline structure similar to that of films obtained through conventional thermal annealing methods. However, the fast pulsed nature of the laser employed leads to crystallization kinetic evolution orders of magnitude faster than inmore » thermal treatments. The combination of specific photothermal and photochemical mechanisms is the main responsible for the ultrafast epitaxial laser-induced crystallization. Piezoresponse microscopy measurements demonstrate equivalent ferroelectric behavior in laser and thermally annealed films, being the piezoelectric constant ∼25 pm V{sup −1}.« less

Utilization of oriented crystal growth for screening of aromatic carboxylic acids cocrystallization with urea

NASA Astrophysics Data System (ADS)

Przybyłek, Maciej; Ziółkowska, Dorota; Kobierski, Mirosław; Mroczyńska, Karina; Cysewski, Piotr

2016-01-01

The possibility of molecular complex formation in the solid state of urea with benzoic acid analogues was measured directly on the crystallite films deposited on the glass surface using powder X-ray diffractometry (PXRD). Obtained solid mixtures were also analyzed using Fourier transform infrared spectroscopy (FTIR). The simple droplet evaporation method was found to be efficient, robust, fast and cost-preserving approach for first stage cocrystal screening. Additionally, the application of orientation effect to cocrystal screening simplifies the analysis due to damping of majority of diffraction signals coming from coformers. During validation phase the proposed approach successfully reproduced both positive cases of cocrystallization (urea:salicylic acid and urea:4-hydroxy benzoic acid) as well as pairs of co-formers immiscible in the solid state (urea:benzoic acid and urea:acetylsalicylic acids). Based on validated approach new cocrystals of urea were identified in complexes with 3-hydroxybenzoic acid, 2,4-dihydroxybenzoic acid, 2,5-dihydroxybenzoic acid, 2,6-dihydroxybenzoic acid and 3,5-dihydroxybenzoic acid. In all cases formation of multicomponent crystal phase was confirmed by the appearance of new reflexes on the diffraction patterns and FTIR absorption band shifts of O-H and N-H groups.

Neodymium(III) Complexes of Dialkylphosphoric and Dialkylphosphonic Acids Relevant to Liquid-Liquid Extraction Systems.

PubMed

Lumetta, Gregg J; Sinkov, Sergey I; Krause, Jeanette A; Sweet, Lucas E

2016-02-15

The complexes formed during the extraction of neodymium(III) into hydrophobic solvents containing acidic organophosphorus extractants were probed by single-crystal X-ray diffractometry, visible spectrophotometry, and Fourier-transform infrared spectroscopy. The crystal structure of the compound Nd(DMP)3 (1, DMP = dimethyl phosphate) revealed a polymeric arrangement in which each Nd(III) center is surrounded by six DMP oxygen atoms in a pseudo-octahedral environment. Adjacent Nd(III) ions are bridged by (MeO)2POO(-) anions, forming the polymeric network. The diffuse reflectance visible spectrum of 1 is nearly identical to that of the solid that is formed when an n-dodecane solution of di(2-ethylhexyl)phosphoric acid (HA) is saturated with Nd(III), indicating a similar coordination environment around the Nd center in the NdA3 solid. The visible spectrum of the HA solution fully loaded with Nd(III) is very similar to that of the NdA3 material, both displaying hypersensitive bands characteristic of an pseudo-octahedral coordination environment around Nd. These spectral characteristics persisted across a wide range of organic Nd concentrations, suggesting that the pseudo-octahedral coordination environment is maintained from dilute to saturated conditions.

Effects of polymer type and storage relative humidity on the kinetics of felodipine crystallization from amorphous solid dispersions.

PubMed

Rumondor, Alfred C F; Stanford, Lindsay A; Taylor, Lynne S

2009-12-01

The objective of this study was to investigate the effects of polymer type and storage relative humidity (RH) on the crystallization kinetics of felodipine from amorphous solid dispersions. Crystallization of the model drug felodipine from amorphous solid dispersion samples containing poly(vinyl pyrrolidone) (PVP) and hypromellose acetate succinate (HPMCAS) were evaluated. Samples at three different drug-polymer weight ratios (10, 25, and 50 wt. % polymer) were prepared and stored at six different RHs (0%, 32%, 52% or 66%, 75%, 86%, and 93%). Periodically, the fraction of the drug that had crystallized from the samples was quantified using powder X-ray diffractometry (PXRD). Felodipine crystallization rates from PVP-containing dispersions were found to be very sensitive to changes in storage RH, while crystallization rates from HPMCAS-containing dispersions were not. PVP and HPMCAS were similar in terms of their ability to inhibit crystallization at low RH, but when the storage RH was increased to 75% or above, felodipine crystallization from PVP-containing solid dispersions proceeded much faster. It is hypothesized that this trend was caused by moisture-induced drug-polymer immiscibility in PVP-felodipine system. For PVP-containing solid dispersion samples stored at 75% RH and above, crystallization of the model drug felodipine seemed to approach a kinetic plateau, whereby a fraction of the drug still remained amorphous even after storage for 500 days or more. The physical stability of solid dispersions as a function of RH is highly dependent on the polymer used to form the solid dispersion, with PVP-containing dispersions being much less physically stable at high RH than HPMCAS-containing dispersions.

All-diamond optical assemblies for a beam-multiplexing X-ray monochromator at the Linac Coherent Light Source

PubMed Central

Stoupin, S.; Terentyev, S. A.; Blank, V. D.; Shvyd’ko, Yu. V.; Goetze, K.; Assoufid, L.; Polyakov, S. N.; Kuznetsov, M. S.; Kornilov, N. V.; Katsoudas, J.; Alonso-Mori, R.; Chollet, M.; Feng, Y.; Glownia, J. M.; Lemke, H.; Robert, A.; Sikorski, M.; Song, S.; Zhu, D.

2014-01-01

A double-crystal diamond (111) monochromator recently implemented at the Linac Coherent Light Source (LCLS) enables splitting of the primary X-ray beam into a pink (transmitted) and a monochromatic (reflected) branch. The first monochromator crystal, with a thickness of ∼100 µm, provides sufficient X-ray transmittance to enable simultaneous operation of two beamlines. This article reports the design, fabrication and X-ray characterization of the first and second (300 µm-thick) crystals utilized in the monochromator and the optical assemblies holding these crystals. Each crystal plate has a region of about 5 × 2 mm with low defect concentration, sufficient for use in X-ray optics at the LCLS. The optical assemblies holding the crystals were designed to provide mounting on a rigid substrate and to minimize mounting-induced crystal strain. The induced strain was evaluated using double-crystal X-ray topography and was found to be small over the 5 × 2 mm working regions of the crystals. PMID:25242912

X-ray Crystallography Facility

NASA Technical Reports Server (NTRS)

2000-01-01

Edward Snell, a National Research Council research fellow at NASA's Marshall Space Flight Center (MSFC), prepares a protein crystal for analysis by x-ray crystallography as part of NASA's structural biology program. The small, individual crystals are bombarded with x-rays to produce diffraction patterns, a map of the intensity of the x-rays as they reflect through the crystal.

Mechanical design of thin-film diamond crystal mounting apparatus for coherence preservation hard x-ray optics

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

Shu, Deming, E-mail: shu@aps.anl.gov; Shvyd’ko, Yuri V.; Stoupin, Stanislav

2016-07-27

A new thin-film diamond crystal mounting apparatus has been designed at the Advanced Photon Source (APS) for coherence preservation hard x-ray optics with optimized thermal contact and minimized crystal strain. This novel mechanical design can be applied to new development in the field of: x-ray optics cavities for hard x-ray free-electron laser oscillators (XFELOs), self-seeding monochromators for hard x-ray free-electron laser (XFEL) with high average thermal loading, high heat load diamond crystal monochromators and beam-sharing/beam-split-and-delay devices for XFEL facilities and future upgraded high-brightness coherent x-ray source in the MBA lattice configuration at the APS.

Correlation Between the Extent of Catalytic Activity and Charge Density of Montmorillonites

PubMed Central

Steudel, Annett; Emmerich, Katja; Lagaly, Gerhard; Schuhmann, Rainer

2010-01-01

Abstract The clay mineral montmorillonite is a member of the phyllosilicate group of minerals, which has been detected on martian soil. Montmorillonite catalyzes the condensation of activated monomers to form RNA-like oligomers. Extent of catalysis, that is, the yield of oligomers, and the length of the longest oligomer formed in these reactions widely varies with the source of montmorillonite (i.e., the locality where the mineral is mined). This study was undertaken to establish whether there exists a correlation between the extent of catalytic property and the charge density of montmorillonites. Charge density was determined by saturating the montmorillonites with alkyl ammonium cations that contained increasing lengths of alkyl chains, [CH3-(CH2)n-NH3]+, where n = 3–16 and 18, and then measuring d(001), interlayer spacing of the resulting montmorillonite-alkyl ammonium-montmorillonite complex by X-ray diffractometry (XRD). Results demonstrate that catalytic activity of montmorillonites with lower charge density is superior to that of higher charge density montmorillonite. They produce longer oligomers that contain 9 to 10 monomer units, while montmorillonite with high charge density catalyzes the formation of oligomers that contain only 4 monomer units. The charge density of montmorillonites can also be calculated from the chemical composition if elemental analysis data of the pure mineral are available. In the next mission to Mars, CheMin (Chemistry and Mineralogy), a combined X-ray diffraction/X-ray fluorescence instrument, will provide information on the mineralogical and elemental analysis of the samples. Possible significance of these results for planning the future missions to Mars for the search of organic compounds and extinct or extant life is discussed. Key Words: Mars—Origin of life—Montmorillonite—Mineral catalysis—Layer charge density—X–ray diffractometry. Astrobiology 10, 743–749. PMID:20854214

Fast ultrasonic wavelength tuning in X-ray experiment

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

Blagov, A. E., E-mail: blagov-ae@mail.ru; Pisarevskii, Yu. V.; Koval’chuk, M. V.

2016-03-15

A method of tuning (scanning) X-ray beam wavelength based on modulation of the lattice parameter of X-ray optical crystal by an ultrasonic standing wave excited in it has been proposed and experimentally implemented. The double-crystal antiparallel scheme of X-ray diffraction, in which an ultrasonic wave is excited in the second crystal, is used in the experiment. The profile of characteristic line k{sub α1} of an X-ray tube with a molybdenum anode is recorded using both the proposed tuning scheme and conventional mechanical rotation of crystal. The results obtained by both techniques are in good agreement.

Nano-Tubular Cellulose for Bioprocess Technology Development

PubMed Central

Koutinas, Athanasios A.; Sypsas, Vasilios; Kandylis, Panagiotis; Michelis, Andreas; Bekatorou, Argyro; Kourkoutas, Yiannis; Kordulis, Christos; Lycourghiotis, Alexis; Banat, Ibrahim M.; Nigam, Poonam; Marchant, Roger; Giannouli, Myrsini; Yianoulis, Panagiotis

2012-01-01

Delignified cellulosic material has shown a significant promotional effect on the alcoholic fermentation as yeast immobilization support. However, its potential for further biotechnological development is unexploited. This study reports the characterization of this tubular/porous cellulosic material, which was done by SEM, porosimetry and X-ray powder diffractometry. The results showed that the structure of nano-tubular cellulose (NC) justifies its suitability for use in “cold pasteurization” processes and its promoting activity in bioprocessing (fermentation). The last was explained by a glucose pump theory. Also, it was demonstrated that crystallization of viscous invert sugar solutions during freeze drying could not be otherwise achieved unless NC was present. This effect as well as the feasibility of extremely low temperature fermentation are due to reduction of the activation energy, and have facilitated the development of technologies such as wine fermentations at home scale (in a domestic refrigerator). Moreover, NC may lead to new perspectives in research such as the development of new composites, templates for cylindrical nano-particles, etc. PMID:22496794

Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

NASA Technical Reports Server (NTRS)

Singer, J.; Fielder, W. L.; Garlick, R. G.; Negas, T.

1987-01-01

NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

Nano-tubular cellulose for bioprocess technology development.

PubMed

Koutinas, Athanasios A; Sypsas, Vasilios; Kandylis, Panagiotis; Michelis, Andreas; Bekatorou, Argyro; Kourkoutas, Yiannis; Kordulis, Christos; Lycourghiotis, Alexis; Banat, Ibrahim M; Nigam, Poonam; Marchant, Roger; Giannouli, Myrsini; Yianoulis, Panagiotis

2012-01-01

Delignified cellulosic material has shown a significant promotional effect on the alcoholic fermentation as yeast immobilization support. However, its potential for further biotechnological development is unexploited. This study reports the characterization of this tubular/porous cellulosic material, which was done by SEM, porosimetry and X-ray powder diffractometry. The results showed that the structure of nano-tubular cellulose (NC) justifies its suitability for use in "cold pasteurization" processes and its promoting activity in bioprocessing (fermentation). The last was explained by a glucose pump theory. Also, it was demonstrated that crystallization of viscous invert sugar solutions during freeze drying could not be otherwise achieved unless NC was present. This effect as well as the feasibility of extremely low temperature fermentation are due to reduction of the activation energy, and have facilitated the development of technologies such as wine fermentations at home scale (in a domestic refrigerator). Moreover, NC may lead to new perspectives in research such as the development of new composites, templates for cylindrical nano-particles, etc.

Hierarchical macro-mesoporous structures in the system TiO{sub 2}-Al{sub 2}O{sub 3}, obtained by hydrothermal synthesis using Tween-20 as a directing agent

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

Garcia-Benjume, M.L.; Espitia-Cabrera, M.I.; Contreras-Garcia, M.E., E-mail: eucontre@zeus.umich.mx

2009-12-15

Macro-mesoporous powders of titania, alumina, and mixed titania-20%alumina systems were obtained by hydrothermal synthesis employing surfactant Tween-20 as structural directing agent in order to promote the textural properties of titania. The effect of the alumina in the titania phase and on textural properties was analyzed. The obtained powders presented a macroporous channel structure that was characterized by X-ray diffractometry, scanning and transmission electron microscopy, N{sub 2} adsorption-desorption analysis, pore size distribution, Fourier transform infrared spectrometry, and thermogravimetric analysis. It was found that alumina content retarded the anatase phase crystallization and increased the Brunauer-Emmet-Teller surface area from 136 to 210 m{supmore » 2}/g. The powders calcined at 400 deg. C are thermally stable and possess an interconnected macro-mesoporous hierarchical structure; the results indicate that this synthesis can be employed to prepare mixed titania-alumina with good textural properties.« less

A mixed valence zinc dithiolene system with spectator metal and reactor ligands.

PubMed

Ratvasky, Stephen C; Mogesa, Benjamin; van Stipdonk, Michael J; Basu, Partha

2016-08-16

Neutral complexes of zinc with N,N'-diisopropylpiperazine-2,3-dithione ( i Pr 2 Dt 0 ) and N,N'-dimethylpiperazine-2,3-dithione (Me 2 Dt 0 ) with chloride or maleonitriledithiolate (mnt 2- ) as coligands have been synthesized and characterized. The molecular structures of these zinc complexes have been determined using single crystal X-ray diffractometry. Complexes recrystallize in monoclinic P type systems with zinc adopting a distorted tetrahedral geometry. Two zinc complexes with mixed-valent dithiolene ligands exhibit ligand-to-ligand charge transfer bands. Optimized geometries, molecular vibrations and electronic structures of charge-transfer complexes were calculated using density functional theory (B3LYP/6-311G+(d,p) level). Redox orbitals are shown to be almost exclusively ligand in nature, with a HOMO based heavily on the electron-rich maleonitriledithiolate ligand, and a LUMO comprised mostly of the electron-deficient dithione ligand. Charge transfer is thus believed to proceed from dithiolate HOMO to dithione LUMO, showing ligand-to-ligand redox interplay across a d 10 metal.

Heteroepitaxial growth of Ge films on (100) GaAs by pyrolysis of digermane

NASA Astrophysics Data System (ADS)

Eres, Djula; Lowndes, Douglas H.; Tischler, J. Z.; Sharp, J. W.; Geohegan, D. B.; Pennycook, S. J.

1989-08-01

Pyrolysis of high-purity digermane (Ge2 H6 ) has been used to grow epitaxial Ge films of high crystalline quality on (100) GaAs substrates in a low-pressure environment. X-ray double-crystal diffractometry shows that fully commensurate, coherently strained epitaxial Ge films can be grown on (100) GaAs at digermane partial pressures of 0.05-40 mTorr for substrate temperatures of 380-600 °C. Amorphous films also were deposited. Information about the crystalline films surface morphology, growth mode, and microstructure was obtained from scanning electron microscopy, cross-section transmission electron microscopy, and in situ reflectivity measurements. The amorphous-to-crystalline transition temperature and the morphology of the crystalline films were both found to depend on deposition conditions (primarily the incidence rate of Ge-bearing species and the substrate temperature). Epitaxial growth rates using digermane were found to be about two orders of magnitude higher than rates using germane (GeH4 ) under similar experimental conditions.

Change Spectrum Characteristics Modification of Films Deposited by Magnetron Sputtering with the Assistance of Argon Ions Beam

NASA Astrophysics Data System (ADS)

Umnov, S.; Asainov, O.

2015-04-01

Thin aluminum films were prepared using the method of magnetron sputtering with and without argon ion beam assistance. The influence of argon ion beam on the reflectivity in the UV range and the structure of aluminum films was studied. The structure of the films was studied by transmission electron microscopy (TEM), X-ray diffractometry (XRD) and atomic- force microscope (AFM). The study has shown that the films deposed with the assistance of the argon ion beam have more significant microstresses associated with an increase of crystallites microstructure defects as compared to the films deposed without ion assistance. Comparison of the measured reflectivity of aluminum films deposed without and with the assistance of the ion beam has shown that the films characterized by a higher level of microstructure def ects have increased reflectivity in the UV range. The studies suggest that the defects of thin aluminum films crystal structure influence its optical properties.

Fine Structure Study of the Plasma Coatings B4C-Ni-P

NASA Astrophysics Data System (ADS)

Kornienko, E. E.; Bezrukova, V. A.; Kuz'min, V. I.; Lozhkin, V. S.; Tutunkova, M. K.

2017-12-01

The article considers structure of coatings formed of the B4C-Ni-P powder. The coatings were deposited using air-plasma spraying with the unit for annular injection of powder. The pipes from steel 20 (0.2 % C) were used as a substrate. The structure and phase composition of the coatings were studied by optical microscopy, scanning electron microscopy, transmission electron microscopy and X-ray diffractometry. It is shown that high-density composite coatings consisting of boron carbide particles distributed in the nickel boride metal matrix are formed using air-plasma spraying. The areas with round inclusions characterized by the increased amount of nickel, phosphorus and boron are located around the boron carbide particles. Boron oxides and nickel oxides are also present in the coatings. Thin interlayers with amorphous-crystalline structure are formed around the boron carbide particles. The thickness of these interlayers does not exceed 1 μm. The metal matrix material represents areas with nanocrystalline structure and columnar crystals.

Compositional homogeneity and X-ray topographic analyses of CdTe xSe 1-x grown by the vertical Bridgman technique

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

Roy, U. N.; Bolotnikov, A. E.; Camarda, G. S.

2015-02-01

We grew CdTe xSe 1-x crystals with nominal Se concentrations of 5%, 7%, and 10% by the vertical Bridgman technique, and evaluated their compositional homogeneity and structural quality at the NSLS’ X-ray fluorescence and white beam X-ray topography beam lines. Both X-ray fluorescence and photoluminescence mapping revealed very high compositional homogeneity of the CdTe xSe 1-x crystals. Here, we noted that those crystals with higher concentrations of Se were more prone to twinning than those with a lower content. The crystals were fairly free from strains and contained low concentrations of sub-grain boundaries and their networks.

Synthesis of magnetic mesoporous metal-organic framework-5 for the effective enrichment of malachite green and crystal violet in fish samples.

PubMed

Zhou, Zhihui; Fu, Yanqing; Qin, Qian; Lu, Xin; Shi, Xianzhe; Zhao, Chunxia; Xu, Guowang

2018-07-27

A novel, magnetic and mesoporous Fe 3 O 4 @PEI-MOF-5 material was synthesized for the effective enrichment of malachite green (MG) and crystal violet (CV) in fish samples. The Fe 3 O 4 @PEI-MOF-5 material was prepared by a facile two-step solvothermal approach in which Fe 3 O 4 @PEI and MOF-5 were connected through chemical bonds. Characterization of the newly synthesized Fe 3 O 4 @PEI-MOF-5 material was performed by Fourier transform infrared spectroscopy, X-ray diffractometry, vibrating sample magnetometry, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis and X-ray photoelectron spectroscopy. This new material was determined to have high magnetization and chemical stability, a large surface area and a distinctive morphology. An effective enrichment and detection method for MG and CV was subsequently developed by combining the Fe 3 O 4 @PEI-MOF-5 material with ultra-high-performance liquid chromatography-tandem mass spectrometry. The linearity ranges of this approach for MG and CV were 1-500ng/mL and 0.25-500ng/mL, respectively, with correlation coefficients (R 2 ) of 0.999. The limits of detection (LODs) of the method for MG and CV were 0.30ng/mL and 0.08ng/mL, respectively, indicating that the Fe 3 O 4 @PEI-MOF-5 material had good adsorption properties for MG and CV. Fe 3 O 4 @PEI-MOF-5 can be expected to also provide efficient enrichment of MG and CV in other complex matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

Enhancement of the dissolution rate and bioavailability of fenofibrate by a melt-adsorption method using supercritical carbon dioxide

PubMed Central

Cha, Kwang-Ho; Cho, Kyung-Jin; Kim, Min-Soo; Kim, Jeong-Soo; Park, Hee Jun; Park, Junsung; Cho, Wonkyung; Park, Jeong-Sook; Hwang, Sung-Joo

2012-01-01

Background: The aim of this study was to enhance the bioavailability of fenofibrate, a poorly water-soluble drug, using a melt-adsorption method with supercritical CO2. Methods: Fenofibrate was loaded onto Neusilin® UFL2 at different weight ratios of fenofibrate to Neusilin UFL2 by melt-adsorption using supercritical CO2. For comparison, fenofibrate-loaded Neusilin UFL2 was prepared by solvent evaporation and hot melt-adsorption methods. The fenofibrate formulations prepared were characterized by differential scanning calorimetry, powder x-ray diffractometry, specific surface area, pore size distribution, scanning electron microscopy, and energy-dispersive x-ray spectrometry. In vitro dissolution and in vivo bioavailability were also investigated. Results: Fenofibrate was distributed into the pores of Neusilin UFL2 and showed reduced crystal formation following adsorption. Supercritical CO2 facilitated the introduction of fenofibrate into the pores of Neusilin UFL2. Compared with raw fenofibrate, fenofibrate from the prepared powders showed a significantly increased dissolution rate and better bioavailability. In particular, the area under the drug concentration-time curve and maximal serum concentration of the powders prepared using supercritical CO2 were 4.62-fold and 4.52-fold greater than the corresponding values for raw fenofibrate. Conclusion: The results of this study highlight the usefulness of the melt-adsorption method using supercritical CO2 for improving the bioavailability of fenofibrate. PMID:23118538

Ultrastructure of selected struvite-containing urinary calculi from dogs.

PubMed

Domingo-Neumann, R A; Ruby, A L; Ling, G V; Schiffman, P S; Johnson, D L

1996-09-01

To elucidate the ultrastructural details of struvite-containing urinary calculi from dogs. 38 specimens were selected from a collection of approximately 13,000 canine urinary calculi: 18 of these were composed entirely of struvite, and 20 consisted of struvite and calcium phosphate (apatite). Qualitative and quantitative analyses of specimens included use of plain and polarized light microscopy, x-ray diffractometry, scanning electron microscopy with backscattered electron imagery, x-ray fluorescence scans, and electron microprobe analysis. 4 textural types were recognized among struvite calculi, and 4 textural types of struvite-apatite calculi were described. Evidences of calculus dissolution were described from 4 calculi studied. The presence of small, well interconnected primary pores in struvite-containing urinary calculi from dogs appears to be a significant factor in determining the possible interaction of calculi with changes in the urine composition. The progress of dissolution from the calculus surface to the calculus interior appears to be largely affected by the primary porosity originally present between crystals forming the calculus framework. Apatite was observed to be more resistant to dissolution than struvite. The prevalence of fine concentric laminations having low porosity, and the common occurrence of apatite among struvite-containing urinary calculi from dogs may be 2 reasons why the efficacy of dietary and medicinal manipulations in dissolving urinary calculi is greater among cats than it is among dogs.

A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies

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

Szlachetko, J.; Institute of Physics, Jan Kochanowski University, 25-406 Kielce; Nachtegaal, M.

2012-10-15

We report on the design and performance of a wavelength-dispersive type spectrometer based on the von Hamos geometry. The spectrometer is equipped with a segmented-type crystal for x-ray diffraction and provides an energy resolution in the order of 0.25 eV and 1 eV over an energy range of 8000 eV-9600 eV. The use of a segmented crystal results in a simple and straightforward crystal preparation that allows to preserve the spectrometer resolution and spectrometer efficiency. Application of the spectrometer for time-resolved resonant inelastic x-ray scattering and single-shot x-ray emission spectroscopy is demonstrated.

Capillary optics for radiation focusing

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

Peurrung, A.J.; Reeder, P.L.; Bliss, M.

Capillary lens technology may ultimately bring benefits to neutron and x-ray-based science like conventional lenses with visible light. Although the technology is not yet 10 years old, these lenses have already had a significant impact in engineering, science, and medicine. Capillary lenses are advantageous when it is desirable to increase the radiation flux at a location without regard to its angular divergence. PNNL has worked to improve the technology in several ways. A single, optimally tapered capillary was manufactured, which allows intensity gains of a factor of 270 for an initially parallel, incident x-ray beam. Feasibility of constructing neutron lensesmore » using {sup 58}Ni (particularly effective at reflecting neutrons) has been explored. Three applications for capillary optics have been identified and studied: neutron telescope, Gandolphi x-ray diffractometry, and neutron radiotherapy. A brief guide is given for determining which potential applications are likely to be helped by capillary optics.« less

Inorganic fullerene-like tungsten disulfide nanocoating for friction reduction of nickel-titanium alloys.

PubMed

Samorodnitzky-Naveh, Gili R; Redlich, Meir; Rapoport, Lev; Feldman, Yishay; Tenne, Reshef

2009-12-01

To fabricate a friction-reducing coating onto different nickel-titanium (NiTi) substrates using inorganic fullerene-like tungsten disulfide (IF-WS(2)) nanoparticles and to estimate in vitro friction reducing extent of the coating. Different NiTi substrates were coated with cobalt and IF-WS(2) nanoparticles film by the electrodeposition procedure. Coating composition analyses was made by scanning-electron microscopy, energy dispersive x-ray spectroscopy, x-ray powder diffractometry and x-ray photoelectron spectroscopy. Friction evaluation was carried out using standard tribological tests and an Instron system. Stable and well-adhered cobalt + IF-WS(2) coating of the NiTi substrates was obtained. Friction tests presented up to 66% reduction of the friction coefficient. NiTi alloy is widely used for many medical appliances; hence, this unique friction-reducing coating could be implemented to provide better manipulation and lower piercing rates.

X-ray rocking curve measurements of bent crystals. [used in High Resolution Spectrometer in Advanced X-ray Astrophysics Facility

NASA Technical Reports Server (NTRS)

Hakim, M. B.; Muney, W. S.; Fowler, W. B.; Woodgate, B. E.

1988-01-01

A three-crystal laboratory X-ray spectrometer is used to measure the Bragg reflection from concave cylindrically curved crystals to be used in the high-resolution X-ray spectrometer of the NASA Advanced X-ray Astrophysics Facility (AXAF). The first two crystals, in the dispersive (1.1) arrangement, select a narrow collimated monochromatic beam in the Cu K-alpha(1) line at 1.5 A (8.1 keV), which illuminates the test crystal. The angular centroids of rocking curves measured along the surface provide a measure of the conformity of the crystal to the desired radius of curvature. Individual and combined rocking-curve widths and areas provide a measure of the resolution and efficiency at 1.54 A. The crystals analyzed included LiF(200), PET, and acid phthalates such as TAP.

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

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

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

2016-07-27

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

Perfectly Cold Crystals: What Happens When They Are X-rayed?

NASA Technical Reports Server (NTRS)

vanderWoerd, Mark; Ferree, Darren S.; Snell, Edward H.

2003-01-01

For many macromolecular crystals the cryo-preservation of these crystals during X-ray data collection is of crucial importance, particularly at synchrotron facilities where the crystals rapidly receive a high dose of radiation. A practical variable to ensure adequate preservation is the variation of the cryo-protectant present when the crystal is preserved. Our initial approach to study X-ray diffraction data quality as a function of cryo-protectant present when preserving a xylose isomerase crystal shows that the data quality can be tremendously improved by recipe adjustment. Guided by crystal mosaicity estimates, we optimized crystal growth conditions to obtain cryo-preserved xylose isomerase crystals that withstand a very high dose of X-rays, with only the smallest amount of radiation damage at ultra-high resolution (1.2Angstroms). The rate at which damage occurs allowed us to collect a series of complete data sets, which show how the data degradation proceeds over time. We are here presenting data for the xylose isomerase crystallization recipe improvement and our interpretation of the crystal degradation process during X-ray data collection.

Syntheses and crystal structures of the rare-earth metal(III) bromide ortho-oxidotungstates(VI) with the formula REBr[WO4] (RE = Y, Gd-Yb)

NASA Astrophysics Data System (ADS)

Schustereit, Tanja; Schleid, Thomas; Hartenbach, Ingo

2015-10-01

The rare-earth metal(III) bromide ortho-oxidotungstates(VI) with the formula REBr[WO4] crystallize triclinically in space group P 1 bar (a = 689-693, b = 715-728, c = 1074-1107 pm, α = 103-106, β ≈ 108 and γ = 93-95°, Z = 4) for RE = Y, Gd-Yb. Their crystal structure is isotypic with the most examples of the formally analogous lanthanoid(III) bromide oxidomolybdates(VI) REBr[MoO4] with RE = Y, Pr, Nd, Sm, Gd-Lu. It contains two crystallographically different rare-earth metal(III) cations with coordination numbers of seven plus one for (RE1)3+ and seven for (RE2)3+. The (RE1)3+ cations are surrounded by three Br- and four plus one O2- anions forming distorted trigonal dodecahedra, while the (RE2)3+ cations exhibit a coordination environment of one Br- and six O2- anions in the shape of a monocapped trigonal prism. Furthermore, the structure contains two crystallographically independent, isolated tetrahedral [WO4]2- units. All these polyhedra are fused together to form 1 ∞ {REBr[WO4]} chains running along [012]. Since the title compounds, synthesized by solid-state reactions from the underlying binaries, emerge as pure phases according to X-ray powder diffractometry, spectroscopic and magnetic measurements were performed.

Spatially resolved single crystal x-ray spectropolarimetry of wire array z-pinch plasmas

NASA Astrophysics Data System (ADS)

Wallace, M. S.; Haque, S.; Neill, P.; Pereira, N. R.; Presura, R.

2018-01-01

A recently developed single-crystal x-ray spectropolarimeter has been used to record paired sets of polarization-dependent and axially resolved x-ray spectra emitted by wire array z-pinches. In this measurement, two internal planes inside a suitable crystal diffract the x-rays into two perpendicular directions that are normal to each other, thereby separating incident x-rays into their linearly polarized components. This paper gives considerations for fielding the instrument on extended sources. Results from extended sources are difficult to interpret because generally the incident x-rays are not separated properly by the crystal. This difficulty is mitigated by using a series of collimating slits to select incident x-rays that propagate in a plane of symmetry between the polarization-splitting planes. The resulting instrument and some of the spatially resolved polarized x-ray spectra recorded for a 1-MA aluminum wire array z-pinch at the Nevada Terawatt Facility at the University of Nevada, Reno will be presented.

Spatially resolved single crystal x-ray spectropolarimetry of wire array z-pinch plasmas.

PubMed

Wallace, M S; Haque, S; Neill, P; Pereira, N R; Presura, R

2018-01-01

A recently developed single-crystal x-ray spectropolarimeter has been used to record paired sets of polarization-dependent and axially resolved x-ray spectra emitted by wire array z-pinches. In this measurement, two internal planes inside a suitable crystal diffract the x-rays into two perpendicular directions that are normal to each other, thereby separating incident x-rays into their linearly polarized components. This paper gives considerations for fielding the instrument on extended sources. Results from extended sources are difficult to interpret because generally the incident x-rays are not separated properly by the crystal. This difficulty is mitigated by using a series of collimating slits to select incident x-rays that propagate in a plane of symmetry between the polarization-splitting planes. The resulting instrument and some of the spatially resolved polarized x-ray spectra recorded for a 1-MA aluminum wire array z-pinch at the Nevada Terawatt Facility at the University of Nevada, Reno will be presented.

Thermophysical properties of carboxylic and amino acid buffers at subzero temperatures: relevance to frozen state stabilization.

PubMed

Sundaramurthi, Prakash; Suryanarayanan, Raj

2011-06-02

Macromolecules and other thermolabile biologicals are often buffered and stored in frozen or dried (freeze-dried) state. Crystallization of buffer components in frozen aqueous solutions and the consequent pH shifts were studied in carboxylic (succinic, malic, citric, tartaric acid) and amino acid (glycine, histidine) buffers. Aqueous buffer solutions were cooled from room temperature (RT) to -25 °C and the pH of the solution was measured as a function of temperature. The thermal behavior of frozen solutions was investigated by differential scanning calorimetry (DSC), and the crystallized phases were identified by X-ray diffractometry (XRD). Based on the solubility of the neutral species of each buffer system over a range of temperatures, it was possible to estimate its degree of supersaturation at the subambient temperature of interest. This enabled us to predict its crystallization propensity in frozen systems. The experimental and the predicted rank orderings were in excellent agreement. The malate buffer system was robust with no evidence of buffer component crystallization and hence negligible pH shift. In the citrate and tartrate systems, at initial pH < pK(a)(2), only the most acidic buffer component (neutral form) crystallized on cooling, causing an increase in the freeze-concentrate pH. In glycine buffer solutions, when the initial pH was ∼3 units < isoelectric pH (pI = 5.9), β-glycine crystallization caused a small decrease in pH, while a similar effect but in the opposite direction was observed when the initial pH was ∼3 units > pI. In the histidine buffer system, depending on the initial pH, either histidine or histidine HCl crystallized.

Supramolecular interactions in biologically relevant compounds. 2-Pyrazineformamide thiosemicarbazones and some products of their cyclization

NASA Astrophysics Data System (ADS)

Castiñeiras, Alfonso; García-Santos, Isabel; Nogueiras, Silvia; Rodríguez-González, Iria; Rodríguez-Riobó, Raúl

2014-09-01

Reaction of 2-cyanopyrazine with thiosemicarbazide or N-methylthiosemicarbazide afforded the (Z)-2-(amino(pyrazin-2-yl)methylene)hydrazinecarbothioamide (HPzAm4DH) and (Z)-2-(amino(pyrazin-2-yl)methylene)-N-methylhydrazine carbothioamide (HPzAm4M), respectively. (2Z,N‧E)-N‧-(4-Oxothiazolidin-2-ylidene)pyrazine-2-carbohydrazonamide (HPzAmot, 5) and (2Z,N‧E)-N‧-(3-methyl-4-oxothiazolidin-2-ylidene)pyrazine-2-carbohydrazonamide (MPzAmot, 7) have been synthesized from these thiosemicarbazones with chloroacetic or bromoacetic acids, using a conventional synthetic methodology and microwave-assisted organic reaction enhancement. The crystal structures of the thiosemicarbazones and their solvates [HPzAm4DHṡ1/2 MeOH (1), HPzAm4DHṡH2O (2), HPzAm4M (3), HPzAm4Mṡ2H2O (4)] and the 1,3-thiazolidin-4-ones (5 and 7) have been studied by X-ray diffractometry. All of the compounds were characterized by elemental analysis, mass spectrometry, FT-IR and 1H and 13C NMR spectroscopy. Several by-products have also been isolated in a crystalline form, namely 3-((Z,E)-N‧-(4-oxothiazolidin-2-ylidene)carbamohydrazonium-yl)pyrazin-1-ium dibromide monohydrate, (H3PzAmot)Br2ṡH2O (6), 2-((5-(pyrazin-2-yl)-1H-1,2,4-triazol-3-yl)thio)acetic acid, (H2Pz124ttAc) (8), 2-amino-5-(pyrazin-2-yl)-1,3,4-thiadiazol-3-ium chloride monohydrate, (HPz134tda)ClṡH2O (9), and 2-(methylamino)-5-(pyrazin-2-yl)-1,3,4-thiadiazol-3-ium chloride N-methyl-5-(pyrazin-2-yl)-1,3,4-thiadiazol-2-amine solvate, (HMPz134tda)Clṡ(MPz134tda) (10). The structures of these compounds were also analyzed by X-ray diffractometry. The microwave-assisted organic reaction method for synthesis is easy, convenient, and ecofriendly when compared to the traditional synthetic methods. Crystal analysis revealed that the compounds have extended 3D supramolecular networks through high levels of H-bonding and weak molecular interactions between the molecular moieties and solvent molecules. The novel synthons, which are sustained by Nsbnd H⋯N and Nsbnd H⋯O hydrogen bonding and other weak interactions, have been shown to assemble with 1,3-thizolidine-4-ones, 1,2,4-trizole, or 1,3,4-thiadiazole derivatives in a zigzag or herringbone architecture.

X-ray Spectropolarimetry of Z-pinch Plasmas with a Single-Crystal Technique

NASA Astrophysics Data System (ADS)

Wallace, Matt; Haque, Showera; Neill, Paul; Pereira, Nino; Presura, Radu

2017-10-01

When directed beams of energetic electrons exist in a plasma the resulting x-rays emitted by the plasma can be partially polarized. This makes plasma x-ray polarization spectroscopy, spectropolarimetry, useful for revealing information about the anisotropy of the electron velocity distribution. X-ray spectropolarimetry has indeed been used for this in both space and laboratory plasmas. X-ray polarization measurements are typically performed employing two crystals, both at a 45° Bragg angle. A single-crystal spectropolarimeter can replace two crystal schemes by utilizing two matching sets of internal planes for polarization-splitting. The polarization-splitting planes diffract the incident x-rays into two directions that are perpendicular to each other and the incident beam as well, so the two sets of diffracted x-rays are linearly polarized perpendicularly to each other. An X-cut quartz crystal with surface along the [11-20] planes and a paired set of [10-10] planes in polarization-splitting orientation is now being used on aluminum z-pinches at the University of Nevada, Reno. Past x-ray polarization measurements have been reserved for point-like sources. Recently a slotted collimating aperture has been used to maintain the required geometry for polarization-splitting enabling the spectropolarimetry of extended sources. The design of a single-crystal x-ray spectropolarimeter and experimental results will be presented. Work was supported by U.S. DOE, NNSA Grant DE-NA0001834 and cooperative agreement DE-FC52-06NA27616.

X-ray structure investigation of some substituted indoles, and the x-ray crystal of 1,1'-bishomocubane

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

Quarles, William G.

1970-05-01

The crystal structures of 5-methoxytryptamine, melatonin, and the p-bromobenzoate of 1,1'-bishomocubane have been solved by x-ray diffraction methods. A computer program for the trial and error solution of crystal structures is also described here.

Well-aligned polycrystalline lanthanum silicate oxyapatite grown by reactive diffusion between solid La{sub 2}SiO{sub 5} and gases [SiO+1/2O{sub 2}

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

Fukuda, Koichiro, E-mail: fukuda.koichiro@nitech.ac.jp; Hasegawa, Ryo; Kitagawa, Takuya

2016-03-15

The c-axis-oriented polycrystalline lanthanum silicate oxyapatite, La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} (□ denotes a vacancy in the Si site), was successfully prepared by the reactive diffusion between randomly grain-oriented La{sub 2}SiO{sub 5} polycrystal and [SiO+1/2O{sub 2}] gases at 1873 K in Ar atmosphere. The polycrystal was characterized using optical microscopy, scanning electron microscopy equipped with energy dispersive X-ray spectroscopy, micro-Raman spectroscopy, X-ray diffractometry, and impedance spectroscopy. The crystal structure (space group P6{sub 3}/m) showed the deficiency of Si site at ca. 1.9%. The bulk oxide-ion conductivity along the grain-alignment direction steadily increased from 9.2 × 10{sup −3} to 1.17 ×more » 10{sup −2} S/cm with increasing temperature from 923 to 1073 K. The activation energy of conduction was 0.23(2) eV. - Graphical abstract: We have successfully prepared the highly c-axis-oriented polycrystalline La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} by the reactive diffusion between randomly grain-oriented La{sub 2}SiO{sub 5} polycrystal and [SiO + 1/2O{sub 2}] gases at 1873 K in Ar atmosphere. The crystal structure (space group P6{sub 3}/m) showed the deficiency of Si site of ca. 1.9%. - Highlights: • The c-axis-oriented polycrystalline La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} is successfully prepared. • Crystal structure of La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} is determined by single-crystal XRD. • The polycrystal shows relatively high oxide ion conductivity along the common c-axis. • Reactive diffusion is successfully used for the preparation of grain-aligned ceramics.« less

Asymmetrically cut crystal pair as x-ray magnifier for imaging at high intensity laser facilitiesa)

NASA Astrophysics Data System (ADS)

Szabo, C. I.; Feldman, U.; Seely, J. F.; Curry, J. J.; Hudson, L. T.; Henins, A.

2010-10-01

The potential of an x-ray magnifier prepared from a pair of asymmetrically cut crystals is studied to explore high energy x-ray imaging capabilities at high intensity laser facilities. OMEGA-EP and NIF when irradiating mid and high Z targets can be a source of high-energy x-rays whose production mechanisms and use as backlighters are a subject of active research. This paper studies the properties and potential of existing asymmetric cut crystal pairs from the National Institute of Standards and Technology (NIST) built in a new enclosure for imaging x-ray sources. The technique of the x-ray magnifier has been described previously. This new approach is aimed to find a design that could be used at laser facilities by magnifying the x-ray source into a screen far away from the target chamber center, with fixed magnification defined by the crystals' lattice spacing and the asymmetry angles. The magnified image is monochromatic and the imaging wavelength is set by crystal asymmetry and incidence angles. First laboratory results are presented and discussed.

Supercrystallization of KCl from solution irradiated by soft X-rays

NASA Astrophysics Data System (ADS)

Janavičius, A. J.; Rinkūnas, R.; Purlys, R.

2016-10-01

The X-rays influence on KCl crystallization in a saturated water solution has been investigated for the aim of comparing it with previously considered NaCl crystallization. The rate of crystallization has been measured in the drying drop in the solution activated by the irradiation. We have measured the influence of the irradiation time of the solution on the rates of KCl crystallization as well as the beginning of the crystallization processes on drying drops. For a longer irradiation time of the solution early crystallization in the drops occurs. A saturated water solution of KCl was irradiated with the diffractometer DRON-3M (Russian device) and this had a great influence on the two-step processes of crystallization. The ionization of the solution by soft X-rays can produce ions, metastable radicals in water, excited crystals' seeds and vacancies in growing crystals by Auger's effect. The X-rays generate a very fast crystallization in the drying drop.

X-ray Microscopic Characterization of Protein Crystals

NASA Technical Reports Server (NTRS)

Hu, Z. W.; Holmes, A.; Thomas, B.R.; Chernov, a. A.; Chu, Y. S.; Lai, B.

2004-01-01

The microscopic mapping of the variation in degree of perfection and in type of defects in entire protein crystals by x-rays may well be a prerequisite for better understanding causes of lattice imperfections, the growth history, and properties of protein crystals. However, x-ray microscopic characterization of bulk protein crystals, in the as-grown state, is frequently more challenging than that of small molecular crystals due to the experimental difficulties arising largely from the unique features possessed by protein crystals. In this presentation, we will illustrate ssme recent activities in employing coherence-based phase contrast x-ray imaging and high-angular-resolution diffraction techniques for mapping microdefects and the degree of perfection of protein crystals, and demonstrate a correlation between crystal perfection, diffraction phenomena., and crystallization conditions. The observed features and phenomena will be discussed in context to gain insight into the nature of defects, nucleation and growth, and the properties of protein crystals.

X-Ray Structure determination of the Glycine Cleavage System Protein H of Mycobacterium tuberculosis Using An Inverse Compton Synchrotron X-Ray Source

PubMed Central

Abendroth, Jan; McCormick, Michael S.; Edwards, Thomas E.; Staker, Bart; Loewen, Roderick; Gifford, Martin; Rifkin, Jeff; Mayer, Chad; Guo, Wenjin; Zhang, Yang; Myler, Peter; Kelley, Angela; Analau, Erwin; Hewitt, Stephen Nakazawa; Napuli, Alberto J.; Kuhn, Peter; Ruth, Ronald D.; Stewart, Lance J.

2010-01-01

Structural genomics discovery projects require ready access to both X-ray and NMR instrumentation which support the collection of experimental data needed to solve large numbers of novel protein structures. The most productive X-ray crystal structure determination laboratories make extensive frequent use of tunable synchrotron X-ray light to solve novel structures by anomalous diffraction methods. This requires that frozen cryo-protected crystals be shipped to large government-run synchrotron facilities for data collection. In an effort to eliminate the need to ship crystals for data collection, we have developed the first laboratory-scale synchrotron light source capable of performing many of the state-of-the-art synchrotron applications in X-ray science. This Compact Light Source is a first-in-class device that uses inverse Compton scattering to generate X-rays of sufficient flux, tunable wavelength and beam size to allow high-resolution X-ray diffraction data collection from protein crystals. We report on benchmarking tests of X-ray diffraction data collection with hen egg white lysozyme, and the successful high-resolution X-ray structure determination of the Glycine cleavage system protein H from Mycobacterium tuberculosis using diffraction data collected with the Compact Light Source X-ray beam. PMID:20364333

Dynamic X-ray diffraction sampling for protein crystal positioning

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

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE PAGES

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; ...

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

PubMed Central

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; Kissick, David J.; Zhang, Shijie; Newman, Justin A.; Sheedlo, Michael J.; Chowdhury, Azhad U.; Fischetti, Robert F.; Das, Chittaranjan; Buzzard, Gregery T.; Bouman, Charles A.; Simpson, Garth J.

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations. PMID:28009558

Dynamic X-ray diffraction sampling for protein crystal positioning.

PubMed

Scarborough, Nicole M; Godaliyadda, G M Dilshan P; Ye, Dong Hye; Kissick, David J; Zhang, Shijie; Newman, Justin A; Sheedlo, Michael J; Chowdhury, Azhad U; Fischetti, Robert F; Das, Chittaranjan; Buzzard, Gregery T; Bouman, Charles A; Simpson, Garth J

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.

Effect of Heat Treatment Temperature on Chemical Compositions of Extracted Hydroxyapatite from Bovine Bone Ash

NASA Astrophysics Data System (ADS)

Younesi, M.; Javadpour, S.; Bahrololoom, M. E.

2011-11-01

This article presents the effect of heat treating temperature on chemical composition of hydroxyapatite (HA) that was produced by burning bovine bone, and then heat treating the obtained bone ash at different temperatures in range of 600-1100 °C in air. Bone ash and the resulting white powder from heat treating were characterized by Fourier transformed infrared spectroscopy (FT-IR) and x-ray diffractometry (XRD). The FT-IR spectra confirmed that heat treating of bone ash at temperature of 800 °C removed the total of organic substances. x-ray diffraction analysis showed that the white powder was HA and HA was the only crystalline phase indicated in heat treating product. x-ray fluorescence analyses revealed that calcium and phosphorous were the main elements and magnesium and sodium were minor impurities of produced powder at 800 °C. The results of the energy dispersive x-ray analysis showed that Ca/P ratio in produced HA varies in range of 1.46-2.01. The resulting material was found to be thermally stable up to 1100 °C.

Multiple wavelength X-ray monochromators

DOEpatents

Steinmeyer, P.A.

1992-11-17

An improved apparatus and method is provided for separating input x-ray radiation containing first and second x-ray wavelengths into spatially separate first and second output radiation which contain the first and second x-ray wavelengths, respectively. The apparatus includes a crystalline diffractor which includes a first set of parallel crystal planes, where each of the planes is spaced a predetermined first distance from one another. The crystalline diffractor also includes a second set of parallel crystal planes inclined at an angle with respect to the first set of crystal planes where each of the planes of the second set of parallel crystal planes is spaced a predetermined second distance from one another. In one embodiment, the crystalline diffractor is comprised of a single crystal. In a second embodiment, the crystalline diffractor is comprised of a stack of two crystals. In a third embodiment, the crystalline diffractor includes a single crystal that is bent for focusing the separate first and second output x-ray radiation wavelengths into separate focal points. 3 figs.

Multiple wavelength X-ray monochromators

DOEpatents

Steinmeyer, Peter A.

1992-11-17

An improved apparatus and method is provided for separating input x-ray radiation containing first and second x-ray wavelengths into spatially separate first and second output radiation which contain the first and second x-ray wavelengths, respectively. The apparatus includes a crystalline diffractor which includes a first set of parallel crystal planes, where each of the planes is spaced a predetermined first distance from one another. The crystalline diffractor also includes a second set of parallel crystal planes inclined at an angle with respect to the first set of crystal planes where each of the planes of the second set of parallel crystal planes is spaced a predetermined second distance from one another. In one embodiment, the crystalline diffractor is comprised of a single crystal. In a second embodiment, the crystalline diffractor is comprised of a stack of two crystals. In a third embodiment, the crystalline diffractor includes a single crystal that is bent for focussing the separate first and second output x-ray radiation wavelengths into separate focal points.

Microgravity

NASA Image and Video Library

2000-04-20

Edward Snell, a National Research Council research fellow at NASA's Marshall Space Flight Center (MSFC), prepares a protein crystal for analysis by x-ray crystallography as part of NASA's structural biology program. The small, individual crystals are bombarded with x-rays to produce diffraction patterns, a map of the intensity of the x-rays as they reflect through the crystal.

X-ray shearing interferometer

DOEpatents

Koch, Jeffrey A [Livermore, CA

2003-07-08

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

Silica nanoparticles produced by DC arc plasma from a solid raw materials

NASA Astrophysics Data System (ADS)

Kosmachev, P. V.; Vlasov, V. A.; Skripnikova, N. K.

2017-05-01

Plasma synthesis of SiO2 nanoparticles in experimental atmospheric pressure plasma reactor on the basis of DC arc plasma generator was presented in this paper. Solid high-silica raw materials such as diatomite from Kamyshlovskoye deposit in Russia, quartzite from Chupinskoye deposit in Russia and milled window glass were used. The obtained nanoparticles were characterized based on their morphology, chemical composition and size distribution. Scanning electron microscopy, laser diffractometry, nitrogen absorption (Brunauer-Emmett-Teller method), X-ray photoelectron spectroscopy and energy-dispersive X-ray spectroscopy were used to characterize the synthesized products. The obtained silica nanoparticles are agglomerated, have spherical shape and primary diameters between 10-300 nm. All samples of synthesized nanopowders were compared with commercial nanopowders.

Synchrotron radiation beamline to study radioactive materials at the Photon Factory

NASA Astrophysics Data System (ADS)

Konishi, Hiroyuki; Yokoya, Akinari; Shiwaku, Hideaki; Motohashi, Haruhiko; Makita, Tomoko; Kashihara, Yasuharu; Hashimoto, Shinya; Harami, Taikan; Sasaki, Teikichi A.; Maeta, Hiroshi; Ohno, Hideo; Maezawa, Hideki; Asaoka, Seiji; Kanaya, Noriichi; Ito, Kenji; Usami, Noriko; Kobayashi, Katsumi

1996-02-01

Design and construction of a new beamline have been described. The beamline is housed in a specially designed area controlled for radioactive materials at the Photon Factory (PF) in the National Laboratory for High Energy Physics (KEK). The beamline system consists of a front-end and two branchlines. One of the branchlines is used for X-ray photoelectron spectroscopy and radiation biology in the energy range of 1.8-6 keV and the other for X-ray diffractometry and XAFS studies as well as radiation biology in the range of 4-20 keV. The former was particularly equipped for the protection against accidental scattering of radioactive materials both inside and outside of the vacuum system.

Characterization of ALD grown TixAlyN and TixAlyC thin films

NASA Astrophysics Data System (ADS)

Kinnunen, S. A.; Malm, J.; Arstila, K.; Lahtinen, M.; Sajavaara, T.

2017-09-01

Atomic layer deposition (ALD) was used to grow TixAlyN and TixAlyC thin films using trimethylaluminum (TMA), titanium tetrachloride and ammonia as precursors. Deposition temperature was varied between 325 °C and 500 °C. Films were also annealed in vacuum and N2-atmosphere at 600-1000 °C. Wide range of characterization methods was used including time-of-flight elastic recoil detection analysis (ToF-ERDA), X-ray diffractometry (XRD), X-ray reflectometry (XRR), Raman spectroscopy, ellipsometry, helium ion microscopy (HIM), atomic force microscopy (AFM) and 4-point probe measurement for resistivity. Deposited films were roughly 100 nm thick and contained mainly desired elements. Carbon, chlorine and hydrogen were found to be the main impurities.

Characterization of the modified nickel-zinc ferrite nanoparticles coated with APTES by salinization reaction

NASA Astrophysics Data System (ADS)

Zainal, Israa G.; Al-Shammari, Ahmed Majeed; Kachi, Wjeah

2018-05-01

Surface functionalization of magnetic iron oxide nanoparticles (NPs) is a kind of functional materials, which have been widely used in the biotechnology and catalysis. In this study, Nickel-Zinc ferrite nanoparticles was functionalized with amino propyl triethoxy silane (APTES) by silanization reaction and both non coated and organosilane-coated magnetite characterized by energy-dispersive X-ray spectroscopy (EDX), X-ray diffractometry, Fourier transformed infrared spectroscopy (FTIR) and atomic force microscopy. Basic groups of amino anchored on the external surface of the coated magnetite were observed. Our study procedure nanoparticles which have surface with free - NH2 groups which can carry out ionic interaction with carboxylic groups and act as a carrier of biological molecules, drugs and metals.

Investigations of interatomic interaction in InAs-InAs1-xSbx heterostructures on a base of x-ray diffractometry

NASA Astrophysics Data System (ADS)

Babjuck, T. I.; Buntar, A. G.; Shevtchuk, L. S.

2001-06-01

Hetero-transitions on a base of InAs and AnSb compounds permitted to obtain cheap light diodes and detectors with the atmosphere maximal transparency region sensibility. There is assumed simultaneously, that the phon radiation in InAs-InAs1-xSbx is not large, which positively effects on receiver parameters. Changing the composition of InAs-InAs1- xSbx solution, one may obtain the structure with the width of forbidden zone of the want of 0.35 to 0,1 eV. There is developed the heterostructures crystalline lattice parameters determining method (for substrate and film) with the DRON-3M x-ray diffractometer. There was found the nonlinear dependence of the heterostructures lattice parameter on the composition. Investigations of interatomic interaction in dependence on composition and also on the forbidden zone width Eg(x) have show, that solid solutions InAs-InAs1- xSbx may be used for the obtaining of infra-red receiver.

Identifying, studying and making good use of macromolecular crystals

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

Calero, Guillermo; Cohen, Aina E.; Luft, Joseph R.

2014-07-25

As technology advances, the crystal volume that can be used to collect useful X-ray diffraction data decreases. The technologies available to detect and study growing crystals beyond the optical resolution limit and methods to successfully place the crystal into the X-ray beam are discussed. Structural biology has contributed tremendous knowledge to the understanding of life on the molecular scale. The Protein Data Bank, a depository of this structural knowledge, currently contains over 100 000 protein structures, with the majority stemming from X-ray crystallography. As the name might suggest, crystallography requires crystals. As detectors become more sensitive and X-ray sources moremore » intense, the notion of a crystal is gradually changing from one large enough to embellish expensive jewellery to objects that have external dimensions of the order of the wavelength of visible light. Identifying these crystals is a prerequisite to their study. This paper discusses developments in identifying these crystals during crystallization screening and distinguishing them from other potential outcomes. The practical aspects of ensuring that once a crystal is identified it can then be positioned in the X-ray beam for data collection are also addressed.« less

Didanosine polymorphism in a supercritical antisolvent process.

PubMed

Bettini, R; Menabeni, R; Tozzi, R; Pranzo, M B; Pasquali, I; Chierotti, M R; Gobetto, R; Pellegrino, L

2010-04-01

Solid-state properties of active ingredients are crucial in pharmaceutical development owing to their significant clinical and economical implications. In the present work we investigated the solid-state properties and the solubility in water of didanosine, DDI, re-crystallized from a dimethylsulfoxide solution using supercritical CO(2) as an antisolvent (SAS process) for comparison with the commercially available drug product. We also applied modern solid-state NMR (SS NMR) techniques, namely 2D (1)H DQ CRAMPS (Combined Rotation And Multiple Pulse Spectroscopy) and (1)H-(13)C on- and off-resonance CP (cross polarization) FSLG-HETCOR experiments, known for providing reliable information about (1)H-(1)H and (1)H-(13)C intra- and intermolecular proximities, in order to address polymorphism issues arising from the crystallization of a new form in the supercritical process. A new polymorph of didanosine was obtained from the supercritical antisolvent process and characterized by means of 1D and 2D multinuclear ((1)H, (13)C, (15)N) SS NMR. The particle size of the new crystal phase was reduced by varying the antisolvent density through a pressure increase. The structural differences between the commercial product and the SAS re-crystallized DDI are highlighted by X-ray diffractometry and well described by solid-state NMR. The carbon C6 (13)C chemical shift suggests that both commercial and re-crystallized didanosine samples are in the enol form. The analysis of homo- and heteronuclear proximities obtained by means of 2D NMR experiments shows that commercial and SAS re-crystallized DDI possess very similar molecular conformation and hydrogen bond network, but different packing. The new polymorph proved to be a metastable form at ambient conditions, showing higher solubility in water and lower stability to mechanical stress. 2009 Wiley-Liss, Inc. and the American Pharmacists Association

Development of speckle-free channel-cut crystal optics using plasma chemical vaporization machining for coherent x-ray applications.

PubMed

Hirano, Takashi; Osaka, Taito; Sano, Yasuhisa; Inubushi, Yuichi; Matsuyama, Satoshi; Tono, Kensuke; Ishikawa, Tetsuya; Yabashi, Makina; Yamauchi, Kazuto

2016-06-01

We have developed a method of fabricating speckle-free channel-cut crystal optics with plasma chemical vaporization machining, an etching method using atmospheric-pressure plasma, for coherent X-ray applications. We investigated the etching characteristics to silicon crystals and achieved a small surface roughness of less than 1 nm rms at a removal depth of >10 μm, which satisfies the requirements for eliminating subsurface damage while suppressing diffuse scattering from rough surfaces. We applied this method for fabricating channel-cut Si(220) crystals for a hard X-ray split-and-delay optical system and confirmed that the crystals provided speckle-free reflection profiles under coherent X-ray illumination.

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

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

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

2008-09-15

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

A comparative study of the luminescence properties of LYSO:Ce, LSO:Ce, GSO:Ce and BGO single crystal scintillators for use in medical X-ray imaging.

PubMed

Valais, I; Michail, C; David, S; Nomicos, C D; Panayiotakis, G S; Kandarakis, I

2008-06-01

The present study is a comparative investigation of the luminescence properties of (Lu,Y)(2)SiO(5):Ce (LYSO:Ce), Lu(2)SiO(5):Ce (LSO:Ce), Gd(2)SiO(5):Ce (GSO:Ce) and (Bi(4)Ge(3)O(12)) BGO single crystal scintillators under medical X-ray excitation. All scintillating crystals have dimensions of 10 x 10 x 10 mm(3) are non-hygroscopic exhibiting high radiation absorption efficiency in the energy range used in medical imaging applications. The comparative investigation was performed by determining the absolute luminescence efficiency (emitted light flux over incident X-ray exposure) in X-ray energies employed in general X-ray imaging (40-140 kV) and in mammographic X-ray imaging (22-49 kV). Additionally, light emission spectra of crystals at various X-ray energies were measured, in order to determine the spectral compatibility to optical photon detectors incorporated in medical imaging systems and the overall efficiency (effective efficiency) of a scintillator-optical detector combination. The light emission performance of LYSO:Ce and LSO:Ce scintillators studied was found very high for X-ray imaging.

An Excel Spreadsheet for a One-Dimensional Fourier Map in X-ray Crystallography

ERIC Educational Resources Information Center

Clegg, William

2004-01-01

The teaching of crystal structure determination with single-crystal X-ray diffraction at undergraduate level faces numerous challenges. Single-crystal X-ray diffraction is used in a vast range of chemical research projects and forms the basis for a high proportion of structural results that are presented to high-school, undergraduate, and graduate…

Systems and methods for detecting an image of an object using multi-beam imaging from an X-ray beam having a polychromatic distribution

DOEpatents

Parham, Christopher A; Zhong, Zhong; Pisano, Etta; Connor, Jr., Dean M

2015-03-03

Systems and methods for detecting an image of an object using a multi-beam imaging system from an x-ray beam having a polychromatic energy distribution are disclosed. According to one aspect, a method can include generating a first X-ray beam having a polychromatic energy distribution. Further, the method can include positioning a plurality of monochromator crystals in a predetermined position to directly intercept the first X-ray beam such that a plurality of second X-ray beams having predetermined energy levels are produced. Further, an object can be positioned in the path of the second X-ray beams for transmission of the second X-ray beams through the object and emission from the object as transmitted X-ray beams. The transmitted X-ray beams can each be directed at an angle of incidence upon one or more crystal analyzers. Further, an image of the object can be detected from the beams diffracted from the analyzer crystals.

Systems and methods for detecting an image of an object by use of an X-ray beam having a polychromatic distribution

DOEpatents

Parham, Christopher; Zhong, Zhong; Pisano, Etta; Connor, Dean; Chapman, Leroy D.

2010-06-22

Systems and methods for detecting an image of an object using an X-ray beam having a polychromatic energy distribution are disclosed. According to one aspect, a method can include detecting an image of an object. The method can include generating a first X-ray beam having a polychromatic energy distribution. Further, the method can include positioning a single monochromator crystal in a predetermined position to directly intercept the first X-ray beam such that a second X-ray beam having a predetermined energy level is produced. Further, an object can be positioned in the path of the second X-ray beam for transmission of the second X-ray beam through the object and emission from the object as a transmitted X-ray beam. The transmitted X-ray beam can be directed at an angle of incidence upon a crystal analyzer. Further, an image of the object can be detected from a beam diffracted from the analyzer crystal.

First Point-Spread Function and X-Ray Phase Contrast Imaging Results with an 88-mm Diameter Single Crystal

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

Lumpkin, A. H.; Garson, A. B.; Anastasio, M. A.

In this study, we report initial demonstrations of the use of single crystals in indirect x-ray imaging with a benchtop implementation of propagation-based (PB) x-ray phase contrast imaging. Based on single Gaussian peak fits to the x-ray images, we observed a four times smaller system point-spread function (PSF) with the 50-μm thick single crystal scintillators than with the reference polycrystalline phosphor/scintillator. Fiber-optic plate depth-of-focus and Al reflective-coating aspects are also elucidated. Guided by the results from the 25-mm diameter crystal samples, we report additionally the first results with a unique 88-mm diameter single crystal bonded to a fiber optic platemore » and coupled to the large format CCD. Both PSF and x-ray phase contrast imaging data are quantified and presented.« less

Investigation on structural and electrical properties of Fe doped ZnO nanoparticles synthesized by solution combustion method

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

Ram, Mast, E-mail: mastram1999@yahoo.com; Bala, Kanchan; Sharma, Hakikat

In the present study, nanoparticles of Fe doped zinc oxide (ZnO) [Zn{sub 1-x}Fe{sub x}O where x=0.0, 0.01, 0.02, 0.03 and 0.05] were prepared by cost effective solution combustion method. The powder X-ray diffractometry confirms the formation of single phase wurtzite structure. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to investigate the micrsostructure of Fe-doped ZnO nanoparticles. The DC electrical conductivity was found to increase with temperature and measurement was carried out in the temperature range of 300-473K. DC electrical conductivity increases with temperature and decreases with Fe doping concentration.

X-ray transparent microfluidic chips for high-throughput screening and optimization of in meso membrane protein crystallization

PubMed Central

Schieferstein, Jeremy M.; Pawate, Ashtamurthy S.; Wan, Frank; Sheraden, Paige N.; Broecker, Jana; Ernst, Oliver P.; Gennis, Robert B.

2017-01-01

Elucidating and clarifying the function of membrane proteins ultimately requires atomic resolution structures as determined most commonly by X-ray crystallography. Many high impact membrane protein structures have resulted from advanced techniques such as in meso crystallization that present technical difficulties for the set-up and scale-out of high-throughput crystallization experiments. In prior work, we designed a novel, low-throughput X-ray transparent microfluidic device that automated the mixing of protein and lipid by diffusion for in meso crystallization trials. Here, we report X-ray transparent microfluidic devices for high-throughput crystallization screening and optimization that overcome the limitations of scale and demonstrate their application to the crystallization of several membrane proteins. Two complementary chips are presented: (1) a high-throughput screening chip to test 192 crystallization conditions in parallel using as little as 8 nl of membrane protein per well and (2) a crystallization optimization chip to rapidly optimize preliminary crystallization hits through fine-gradient re-screening. We screened three membrane proteins for new in meso crystallization conditions, identifying several preliminary hits that we tested for X-ray diffraction quality. Further, we identified and optimized the crystallization condition for a photosynthetic reaction center mutant and solved its structure to a resolution of 3.5 Å. PMID:28469762

X-ray Diffraction Crystal Calibration and Characterization

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

Michael J. Haugh; Richard Stewart; Nathan Kugland

2009-06-05

National Security Technologies’ X-ray Laboratory is comprised of a multi-anode Manson type source and a Henke type source that incorporates a dual goniometer and XYZ translation stage. The first goniometer is used to isolate a particular spectral band. The Manson operates up to 10 kV and the Henke up to 20 kV. The Henke rotation stages and translation stages are automated. Procedures have been developed to characterize and calibrate various NIF diagnostics and their components. The diagnostics include X-ray cameras, gated imagers, streak cameras, and other X-ray imaging systems. Components that have been analyzed include filters, filter arrays, grazing incidencemore » mirrors, and various crystals, both flat and curved. Recent efforts on the Henke system are aimed at characterizing and calibrating imaging crystals and curved crystals used as the major component of an X-ray spectrometer. The presentation will concentrate on these results. The work has been done at energies ranging from 3 keV to 16 keV. The major goal was to evaluate the performance quality of the crystal for its intended application. For the imaging crystals we measured the laser beam reflection offset from the X-ray beam and the reflectivity curves. For the curved spectrometer crystal, which was a natural crystal, resolving power was critical. It was first necessary to find sources of crystals that had sufficiently narrow reflectivity curves. It was then necessary to determine which crystals retained their resolving power after being thinned and glued to a curved substrate.« less

Development of X-ray spectroscopic polarimetry with bent Si crystals and CFRP substrate

NASA Astrophysics Data System (ADS)

Iizuka, Ryo; Izumiya, Takanori; Tsuboi, Yohko

2016-07-01

The light from celestial objects includes four important quantities; images, time variation, energy spectrum, and polarization. In the field of X-ray astronomy, the capabilities of the former three have remarkably developed. On the other hand, the progress for the polarimetry is considerably delayed because of technical difficulties. In order to make a breakthrough in the field of X-ray polarimetry, we have developed a new type of optics for X-ray polarimetry. The system is collecting Bragg crystal with large area and very high sensitivity for the polarization dedicated to Fe-K lines. We adopt the 400 re ection of Si(100) crystals with high sensitivity for the polarization around Fe-K lines (6 7 keV), and bent the crystals with the wide X-ray band and high S/N ratio. Furthermore, to install small area of CCD to non-focal plane, it also has the spectroscopic capability with the better resolution than that of general X-ray CCD. Our previous development was to bent Si crystals to the cylindrical shape of circle and parabola with the DLC deposition. However, for the better optics for the X-ray polarimetry, the shape should be the paraboloid of revolution to collect X-rays with high S/N ratio. We searched for the method to bent the Si crystals to the shape of the paraboloid of revolution. We devised the method to mold the crystal and the CFRP substrate simultaneously pushed to the sophisticated foundation with the paraboloid of revolution. We developed the prototype of about 8 inch in radius of one-quater size. The crystals was also bent in the circumferential direction. Therefore, the image capability examined with optical parallel beam is 0.6 degree. In this thesis, we discussed the new design for X-ray spectroscopic polarimetry, the evaluation of image capability.

X-ray crystallography

NASA Technical Reports Server (NTRS)

2001-01-01

X-rays diffracted from a well-ordered protein crystal create sharp patterns of scattered light on film. A computer can use these patterns to generate a model of a protein molecule. To analyze the selected crystal, an X-ray crystallographer shines X-rays through the crystal. Unlike a single dental X-ray, which produces a shadow image of a tooth, these X-rays have to be taken many times from different angles to produce a pattern from the scattered light, a map of the intensity of the X-rays after they diffract through the crystal. The X-rays bounce off the electron clouds that form the outer structure of each atom. A flawed crystal will yield a blurry pattern; a well-ordered protein crystal yields a series of sharp diffraction patterns. From these patterns, researchers build an electron density map. With powerful computers and a lot of calculations, scientists can use the electron density patterns to determine the structure of the protein and make a computer-generated model of the structure. The models let researchers improve their understanding of how the protein functions. They also allow scientists to look for receptor sites and active areas that control a protein's function and role in the progress of diseases. From there, pharmaceutical researchers can design molecules that fit the active site, much like a key and lock, so that the protein is locked without affecting the rest of the body. This is called structure-based drug design.

Radiation of X-Rays Using Uniaxially Polarized LiNbO3 Single Crystal

NASA Astrophysics Data System (ADS)

Fukao, Shinji; Nakanishi, Yoshikazu; Mizoguchi, Tadahiro; Ito, Yoshiaki; Nakamura, Toru; Yoshikado, Shinzo

2009-03-01

X-rays are radiated due to the bremsstrahlung caused by the collision of electrons with a metal target placed opposite the negative electric surface of a crystal by changing the temperature of a LiNbO3 single crystal uniaxially polarized in the c-axis direction. It is suggested that both electric field intensity and electron density determine the intensity of X-ray radiation. Electrons are supplied by the ionization of residual gas in space, field emission from a case inside which a crystal is located, considered to be due to the high electric-field intensity formed by the surface charges on the crystal, and an external electron source, such as a thermionic source. In a high vacuum, it was found that the electrons supplied by electric-field emission mainly contribute to the radiation of X-rays. It was found that the integrated intensity of X-rays can be maximized by supplying electrons both external and by electric-field emission. Furthermore, the integrated intensity of the X-rays is stable for many repeated temperature changes.

Systematic search for spherical crystal X-ray microscopes matching 1–25 keV spectral line sources

DOE PAGES

Schollmeier, Marius S.; Loisel, Guillaume P.

2016-12-29

Spherical-crystal microscopes are used as high-resolution imaging devices for monochromatic x-ray radiography or for imaging the source itself. Crystals and Miller indices (hkl) have to be matched such that the resulting lattice spacing d is close to half the spectral wavelength used for imaging, to fulfill the Bragg equation with a Bragg angle near 90° which reduces astigmatism. Only a few suitable crystal and spectral-line combinations have been identified for applications in the literature, suggesting that x-ray imaging using spherical crystals is constrained to a few chance matches. In this paper, after performing a systematic, automated search over more thanmore » 9 × 10 6 possible combinations for x-ray energies between 1 and 25 keV, for six crystals with arbitrary Miller-index combinations hkl between 0 and 20, we show that a matching, efficient crystal and spectral-line pair can be found for almost every He α or K α x-ray source for the elements Ne to Sn. Finally, using the data presented here it should be possible to find a suitable imaging combination using an x-ray source that is specifically selected for a particular purpose, instead of relying on the limited number of existing crystal imaging systems that have been identified to date.« less

An x-ray diffraction study of microstructural deformation induced by cyclic loading of selected steels

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

Fourspring, P.M.; Pangborn, R.N.

1997-12-31

X-ray double crystal diffractometry (XRDCD) was used to assess cyclic microstructural deformation in a face centered cubic (fcc) steel (AISI304) and a body centered cubic (bcc) steel (SA508 class 2). The objectives of the investigation were to determine if XRDCD could be used effectively to monitor cyclic microstructural deformation in polycrystalline Fe alloys and to study the distribution of the microstructural deformation induced by cyclic loading in these alloys. The approach used in the investigation was to induce fatigue damage in a material and to characterize the resulting microstructural deformation at discrete fractions of the fatigue life of the material.more » Also, characterization of microstructural deformation was carried out to identify differences in the accumulation of damage from the surface to the bulk, focusing on the following three regions: near surface (0--10 {micro}m), subsurface (10--300 {micro}m), and bulk. Characterization of the subsurface region was performed only on the AISI304 material because of the limited availability of the SA508 material. The results from the XRDCD data indicate a measurable change induced by fatigue from the initial state to subsequent states of both the AISI304 and the SA508 materials. Therefore, the XRDCD technique was shown to be sensitive to the microstructural deformation caused by fatigue in steels; thus, the technique can be used to monitor fatigue damage in steels.« less

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

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

Stoupin, Stanislav; Antipov, Sergey; Butler, James E.

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 configurationmore » and data analysis using rocking-curve topography. In conclusion, 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.« less

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

PubMed

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.

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

DOE PAGES

Stoupin, Stanislav; Antipov, Sergey; Butler, James E.; ...

2016-08-10

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 configurationmore » and data analysis using rocking-curve topography. In conclusion, 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.« less

X-ray reciprocal space mapping of dislocation-mediated strain relaxation during InGaAs/GaAs(001) epitaxial growth

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

Sasaki, Takuo; Ohshita, Yoshio; Kamiya, Itaru

2011-12-01

Dislocation-mediated strain relaxation during lattice-mismatched InGaAs/GaAs(001) heteroepitaxy was studied through in situ x-ray reciprocal space mapping (in situ RSM). At the synchrotron radiation facility SPring-8, a hybrid system of molecular beam epitaxy and x-ray diffractometry with a two-dimensional detector enabled us to perform in situ RSM at high-speed and high-resolution. Using this experimental setup, four results in terms of film properties were simultaneously extracted as functions of film thickness. These were the lattice constants, the diffraction broadenings along in-plane and out-of-plane directions, and the diffuse scattering. Based on correlations among these results, the strain relaxation processes were classified into fourmore » thickness ranges with different dislocation behavior. In addition, the existence of transition regimes between the thickness ranges was identified. Finally, the dominant dislocation behavior corresponding to each of the four thickness ranges and transition regimes was noted.« less

Microgravity

NASA Image and Video Library

2001-06-06

X-rays diffracted from a well-ordered protein crystal create sharp patterns of scattered light on film. A computer can use these patterns to generate a model of a protein molecule. To analyze the selected crystal, an X-ray crystallographer shines X-rays through the crystal. Unlike a single dental X-ray, which produces a shadow image of a tooth, these X-rays have to be taken many times from different angles to produce a pattern from the scattered light, a map of the intensity of the X-rays after they diffract through the crystal. The X-rays bounce off the electron clouds that form the outer structure of each atom. A flawed crystal will yield a blurry pattern; a well-ordered protein crystal yields a series of sharp diffraction patterns. From these patterns, researchers build an electron density map. With powerful computers and a lot of calculations, scientists can use the electron density patterns to determine the structure of the protein and make a computer-generated model of the structure. The models let researchers improve their understanding of how the protein functions. They also allow scientists to look for receptor sites and active areas that control a protein's function and role in the progress of diseases. From there, pharmaceutical researchers can design molecules that fit the active site, much like a key and lock, so that the protein is locked without affecting the rest of the body. This is called structure-based drug design.

Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals

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

Frank, Matthias; Carlson, David B.; Hunter, Mark

2014-02-28

Here we present femtosecond x-ray diffraction patterns from two-dimensional (2-D) protein crystals using an x-ray free electron laser (XFEL). To date it has not been possible to acquire x-ray diffraction from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permits a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy methodology at the Linac Coherent Light Source, we observed Bragg diffraction to better than 8.5 Å resolution for two different 2-D protein crystal samples that were maintained at room temperature. These proof-of-principle results show promisemore » for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.« less

Growth and luminescent properties of Yb:YAG and Ca co-doped Yb:YAG ultrafast scintillation crystals

NASA Astrophysics Data System (ADS)

Zhu, Maodong; Qi, Hongji; Pan, Mingyan; Hou, Qing; Jiang, Benxue; Jin, Yaxue; Han, Hetong; Song, Zhaohui; Zhang, Hui

2018-05-01

In this work, Yb-doped Y3Al5O12 [yttrium aluminum garnet (YAG)] crystals and Ca co-doped Yb:YAG crystals were grown by the Czochralski (CZ) method. The chemical formulas of the two crystals are (Yb0.1Y0.9)3Al5O12 and (Ca0.001Yb0.1Y0.899)3Al5O12, respectively. The structural, optical and luminescent properties of the Yb:YAG and Ca, Yb:YAG crystals were investigated by X-ray rocking curve, X-ray diffraction, Raman spectra, UV-Visble-NIR absorption spectra and X-ray fluorescence. X-ray fluorescence spectrum with two emission peaks at 330 nm and 490 nm were observed in the two kinds of crystals, which would increase slightly after the annealing. Comparing to the Yb:YAG crystal, Ca co-doped Yb:YAG crystal behaved the better luminescent intensity without changing the crystal structure and vibrational modes. This indicates that by doping Ca2+ in Yb:YAG crystal may be an appropriate way to enhance the luminescent property of the scintillation crystal.

Quantitative determination of airborne respirable non-fibrous alpha-silicon carbide by x-ray powder diffractometry.

PubMed

Bye, E; Føreland, S; Lundgren, L; Kruse, K; Rønning, R

2009-06-01

The purpose of the present investigation was to establish a method for the determination of airborne respirable non-fibrous silicon carbide (SiC). The main application is within the industrial production of SiC. Due to the complex airborne aerosol mixture of crystalline compounds in the SiC industry, X-ray powder diffractometry was selected as the most appropriate method. Without any international standard material for the respirable fraction of non-fibrous SiC, pure and suitable products from three SiC plants in Norway were selected. These products have a median particle diameter in the range 4.4-5.1 mum. The method is based on thin sample technique, with the dust deposited on a polycarbonate filter. Absorption correction is done by standard procedures with the use of a silver filter, situated below the polycarbonate filter. The diffraction line used for quantitative determination was selected carefully. This was done to avoid interferences from quartz, cristobalite, and graphite, which all are airborne components present in the atmosphere during the industrial process. The instrumental limit of detection for the method is 12 microg. This method has been used to determine airborne non-fibrous SiC in a comprehensive ongoing project in the Norwegian SiC industry for further epidemiological studies. The method is fully applicable for compliance work.

On the evaluation of the absolute photon energy of Cu Kα, β lines using 4-crystal X -ray spectrometer

NASA Astrophysics Data System (ADS)

Ito, Yoshiaki; Tochio, Tatsunori; Fukushima, Sei

A 4-crystal X-ray spectrometer was designed based on a 2-crystal X-ray spectrometer to be able to perform the absolute measurement of Bragg angle. This basic thought based on 2 crystals dates back to the times to A.Compton etc.. Because a distortion to give the crystal by the adhesive when a crystal was glued, greatly affected the X-rays profile, we changed it to the channel cut crystal without a free distortion as for having made each crystal of 2-crystal a channel cut. The influence of the foot in the spectral profile is more suppressed because four times of reflections reflect it. It is a high resolution so as not to need to consider instrumental function by the reflection degree that a specific atomic analysis can be executed with the chemical state which it is possible for making the placement of the 4-crystal (+, +) setting. This type of spectrum device is first time in the world. Because the absolute measurement of 2 θ angles is enabled by (+,-) and (+, +) setting from the center of gravity position of the rocking curve and the center of gravity position of the X-rays spectrum, we may measure the absolute value of the X-ray photon energy. Because we evaluated the energy of the Cu Kα , β lines, we report it. We acknowledge financial support for the measurements of a part of the data by the REXDAB collaboration that was initiated within the International Fundamental Parameter Initiative.

Triaxial Measurement Method for Analysis of Residual Stress after High Feed Milling by X-Ray Diffraction

NASA Astrophysics Data System (ADS)

Čuma, Matúš; Török, Jozef; Telišková, Monika

2016-12-01

Surface integrity is a broad term which includes various quality factors affecting the functional properties of parts. Residual stress is one of these factors. Machining generates residual stresses in the surface and subsurface layers of the structural elements. X-ray diffractometry is a non-destructive method applicable for the measurement of residual stresses in surface and subsurface layers of components. The article is focused on the non-destructive progressive method of triaxial measurement of residual stress after machining the surface of sample by high feed milling technology. Significance of triaxial measuring is the capability of measuring in different angles so it is possible to acquire stress tensor containing normal and shear stress components acting in the spot of measuring, using a Cartesian coordinate system.

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

Sundaramurthi, Prakash; Suryanarayanan, Raj

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

Analysis of Short and Long Range Atomic Order in Nanocrystalline Diamonds with Application of Powder Diffractometry

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Neuefiend, J.; Weber, H.-P.; Proffen, T.; VonDreele, R.; Palosz, W.;

Fundamentals of Passive Oxidation In SiC and Si3N4

NASA Technical Reports Server (NTRS)

Thomas-Ogbuji, Linus U.

1998-01-01

The very slow oxidation kinetics of silicon carbide and silicon nitride, which derive from their adherent and passivating oxide films, has been explored at length in a broad series of studies utilizing thermogravimetric analysis, electron and optical micrography, energy dispersive spectrometry, x-ray diffractometry, micro-analytical depth profiling, etc. Some interesting microstructural phenomena accompanying the process of oxidation in the two materials will be presented. In Si3N4 the oxide is stratified, with an SiO2 topscale (which is relatively impervious to O2)underlain by a coherent subscale of silicon oxynitride which is even less permeable to O2- Such "defence in depth" endows Si3N4 with what is perhaps the highest oxidation resistance of any material, and results in a unique set of oxidation processes. In SiC the oxidation reactions are much simpler, yet new issues still emerge; for instance, studies involving controlled devitrification of the amorphous silica scale confirmed that the oxidation rate of SiC drops by more than an order of magnitude when the oxide scale fully crystallizes.

Stimulation of processes of self-propagating high temperature synthesis in system Ti + Al at low temperatures by influence of γ-quanta

NASA Astrophysics Data System (ADS)

Sobachkin, A. V.; Loginova, M. V.; Sitnikov, A. A.; Yakovlev, V. I.; Filimonov, V. Yu; Gradoboev, A. V.

2018-03-01

In the present work, the influence of the irradiation with gamma-quanta 60Co upon the structural and phase state of the components of the mechanically activated powder composition of Ti+Al is investigated. The phase composition, structural parameters, and crystallinity are examined by means of X-ray diffractometry. It is found out that the irradiation with gamma-quanta changes the structure of the mechanically activated powder composition. The higher irradiation dose, the higher the structure crystallinity of both components with no change in phase state. At the same time, the parameters of Ti and Al crystal lattices approach to the initial parameters observed before the mechanical activation. The irradiation with gammaquanta leads to decrease of internal stresses in the mechanically activated powder composition while nanocrystallinity of the structure remains unchanged. Using of powder compositions exposed to the irradiation with gamma-quanta for the SH-synthesis helps to increase speed of the reaction, decrease the peak firing temperature and improve homogeneity, as well as the main phase of the produced material is TiAl.

Rivastigmine hydrogen tartrate polymorphs: Solid-state characterisation of transition and polymorphic conversion via milling

NASA Astrophysics Data System (ADS)

Amaro, Maria Inês; Simon, Alice; Cabral, Lúcio Mendes; de Sousa, Valéria Pereira; Healy, Anne Marie

2015-11-01

Rivastigmine (RHT) is an active pharmaceutical ingredient that is used for the treatment of mild to moderately severe dementia in Alzheimer's disease, and is known to present two polymorphic forms and to amorphise upon granulation. To date there is no information in the scientific or patent literature on polymorphic transition and stability. Hence, the aim of the current study was to gain a fundamental understanding of the polymorphic forms by (1) evaluating RHT thermodynamic stability (monotropy or enantiotropy) and (2) investigating the potential for polymorphic transformation upon milling. The two polymorphic and amorphous forms were characterised using X-ray powder diffractometry, thermal analyses, infra-red spectroscopy and water sorption analysis. The polymorphic transition was found to be spontaneous (ΔG0 < 0) and exothermic (ΔH0 < 0), indicative of a monotropic polymorph pair. The kinetic studies showed a fast initial polymorphic transition characterised by a heterogeneous nucleation, followed by a slow crystal growth. Ball milling can be used to promote the polymorphic transition and for the production of RHT amorphous form.

The Effect of Sugarcane Bagassès Size on the Properties of Pretreatment and Enzymatic Hydrolysis

NASA Astrophysics Data System (ADS)

Xu, Jun; Zhou, Guoqiang; Li, Jun

2017-06-01

The influence of milled bagasse particle size on their reducing sugar and lignin content during dilute acid hydrolysis followed by enzymolysis was investigated. The biomass crystal structures of hydrolyzed residues and enzymolyzed substrates were studied with X-ray diffractometry (XRD). The results showed that the conversion ratio of reducing sugar declined with decreasing milled bagasse particle size. The conversion ratio of reducing sugar after acid hydrolysis decreased from 31.3% to 28.9%. The smaller of the milled bagasse particle size was, the higher of the klason lignin content of hydrolyzed residuals was, which resulted in a decline in conversion ratio of reducing sugar during enzymolysis. In this study, the optimal size of milled bagasse particles was 10 to 20 meshes. The total reducing sugar conversion ratio was 61.5%, consisting of 31.3% in hydrolysis and 30.2% in enzymolysis. After hydrolysis, the specific surface area and pore size increased, and the fiber length was shortened. The inner microfiber bundles were exposed, which improved the accessibility of cellulase and the efficiency of enzymolysis.

Multilayer and grazing incidence X-ray/EUV optics; Proceedings of the Meeting, San Diego, CA, July 22-24, 1991

NASA Technical Reports Server (NTRS)

Hoover, Richard B. (Editor)

1992-01-01

The present conference discusses the Advanced X-ray Astrophysics Facility (AXAF) calibration by means of synchrotron radiation and its X-ray reflectivity, X-ray scattering measurements from thin-foil X-ray mirrors, lobster-eye X-ray optics using microchannel plates, space-based interferometry at EUV and soft X-ray wavelengths, a water-window imaging X-ray telescope, a graded d-spacing multilayer telescope for high energy X-ray astronomy, photographic films for the multispectral solar telescope array, a soft X-ray ion chamber, and the development of hard X-ray optics. Also discussed are X-ray spectroscopy with multilayered optics, a slit aperture for monitoring X-ray experiments, an objective double-crystal spectrometer, a Ly-alpha coronagraph/polarimeter, tungsten/boron nitride multilayers for XUV optical applications, the evaluation of reflectors for soft X-ray optics, the manufacture of elastically bent crystals and multilayer mirrors, and selective photodevices for the VUV.

The effect of laser radiation on the diffraction of X-rays in crystals

NASA Astrophysics Data System (ADS)

Trushin, V. N.; Chuprunov, E. V.; Khokhlov, A. F.

1988-10-01

The effect of laser radiation on the intensity of the X-ray diffraction peaks of KDP, ADP, and CuSO4-5H2O crystals was studied experimentally. This intensity was found to increase as a function of the laser beam power. This result suggests that it is possible to use laser beams to control X-ray intensity in the crystals considered.

Application of X-ray topography to USSR and Russian space materials science

PubMed Central

Shul’pina, I. L.; Prokhorov, I. A.; Serebryakov, Yu. A.; Bezbakh, I. Zh.

2016-01-01

The authors’ experience of the application of X-ray diffraction imaging in carrying out space technological experiments on semiconductor crystal growth for the former USSR and for Russia is reported, from the Apollo–Soyuz programme (1975) up to the present day. X-ray topography was applied to examine defects in crystals in order to obtain information on the crystallization conditions and also on their changes under the influence of factors of orbital flight in space vehicles. The data obtained have promoted a deeper understanding of the conditions and mechanisms of crystallization under both microgravity and terrestrial conditions, and have enabled the elaboration of terrestrial methods of highly perfect crystal growth. The use of X-ray topography in space materials science has enriched its methods in the field of digital image processing of growth striations and expanded its possibilities in investigating the inhomogeneity of crystals. PMID:27158506

Observation of divergent-beam X-ray diffraction from a crystal of diamond using synchrotron radiation.

PubMed

Glazer, A M; Collins, S P; Zekria, D; Liu, J; Golshan, M

2004-03-01

In 1947 Kathleen Lonsdale conducted a series of experiments on X-ray diffraction using a divergent beam external to a crystal sample. Unlike the Kossel technique, where divergent X-rays are excited by the presence of fluorescing atoms within the crystal, the use of an external divergent source made it possible to study non-fluorescing crystals. The resulting photographs not only illustrated the complexity of X-ray diffraction from crystals in a truly beautiful way, but also demonstrated unprecedented experimental precision. This long-forgotten work is repeated here using a synchrotron radiation source and, once again, considerable merit is found in Lonsdale's technique. The results of this experiment suggest that, through the use of modern 'third-generation' synchrotron sources, divergent-beam diffraction could soon enjoy a renaissance for high-precision lattice-parameter determination and the study of crystal perfection.

Application of X-ray topography to USSR and Russian space materials science.

PubMed

Shul'pina, I L; Prokhorov, I A; Serebryakov, Yu A; Bezbakh, I Zh

2016-05-01

The authors' experience of the application of X-ray diffraction imaging in carrying out space technological experiments on semiconductor crystal growth for the former USSR and for Russia is reported, from the Apollo-Soyuz programme (1975) up to the present day. X-ray topography was applied to examine defects in crystals in order to obtain information on the crystallization conditions and also on their changes under the influence of factors of orbital flight in space vehicles. The data obtained have promoted a deeper understanding of the conditions and mechanisms of crystallization under both microgravity and terrestrial conditions, and have enabled the elaboration of terrestrial methods of highly perfect crystal growth. The use of X-ray topography in space materials science has enriched its methods in the field of digital image processing of growth striations and expanded its possibilities in investigating the inhomogeneity of crystals.

X-ray transparent Microfluidics for Protein Crystallization and Biomineralization

NASA Astrophysics Data System (ADS)

Opathalage, Achini

Protein crystallization demands the fundamental understanding of nucleation and applying techniques to find the optimal conditions to achieve the kinetic pathway for a large and defect free crystal. Classical nucleation theory predicts that the nucleation occurs at high supersaturation conditions. In this dissertation we sought out to develop techniques to attain optimal supersaturation profile to a large defect free crystal and subject it to in-situ X-ray diffraction using microfluidics. We have developed an emulsion-based serial crystallographic technology in nanolitre-sized droplets of protein solution encapsulated in to nucleate one crystal per drop. Diffraction data are measured, one crystal at a time, from a series of room temperature crystals stored on an X-ray semi-transparent microfluidic chip, and a 93% complete data set is obtained by merging single diffraction frames taken from different un-oriented crystals. As proof of concept, the structure of Glucose Isomerase was solved to 2.1 A. We have developed a suite of X-ray semi-transparent micrfluidic devices which enables; controlled evaporation as a method of increasing supersaturation and manipulating the phase space of proteins and small molecules. We exploited the inherently high water permeability of the thin X-ray semi-transparent devices as a mean of increasing the supersaturation by controlling the evaporation. We fabricated the X-ray semi-transparent version of the PhaseChip with a thin PDMS membrane by which the storage and the reservoir layers are separated, and studies the phase transition of amorphous CaCO3.

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

PubMed

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

2013-10-01

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

Graphene as a protein crystal mounting material to reduce background scatter

PubMed Central

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

2013-01-01

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

Dynamical effects in Bragg coherent x-ray diffraction imaging of finite crystals

NASA Astrophysics Data System (ADS)

Shabalin, A. G.; Yefanov, O. M.; Nosik, V. L.; Bushuev, V. A.; Vartanyants, I. A.

2017-08-01

We present simulations of Bragg coherent x-ray diffractive imaging (CXDI) data from finite crystals in the frame of the dynamical theory of x-ray diffraction. The developed approach is based on a numerical solution of modified Takagi-Taupin equations and can be applied for modeling of a broad range of x-ray diffraction experiments with finite three-dimensional crystals of arbitrary shape also in the presence of strain. We performed simulations for nanocrystals of a cubic and hemispherical shape of different sizes and provided a detailed analysis of artifacts in the Bragg CXDI reconstructions introduced by the dynamical diffraction. Based on our theoretical analysis we developed an analytical procedure to treat effects of refraction and absorption in the reconstruction. Our results elucidate limitations for the kinematical approach in the Bragg CXDI and suggest a natural criterion to distinguish between kinematical and dynamical cases in coherent x-ray diffraction on a finite crystal.

Chemical speciation using high energy resolution PIXE spectroscopy in the tender X-ray range

NASA Astrophysics Data System (ADS)

Kavčič, Matjaž; Petric, Marko; Vogel-Mikuš, Katarina

2018-02-01

High energy resolution X-ray emission spectroscopy employing wavelength dispersive (WDS) crystal spectrometers can provide energy resolution on the level of core-hole lifetime broadening of the characteristic emission lines. While crystal spectrometers have been traditionally used in combination with electron excitation for major and minor element analysis, they have been rarely considered in proton induced X-ray emission (PIXE) trace element analysis mainly due to low detection efficiency. Compared to the simplest flat crystal WDS spectrometer the efficiency can be improved by employing cylindrically or even spherically curved crystals in combination with position sensitive X-ray detectors. When such spectrometer is coupled to MeV proton excitation, chemical bonding effects are revealed in the high energy resolution spectra yielding opportunity to extend the analytical capabilities of PIXE technique also towards chemical state analysis. In this contribution we will focus on the high energy resolution PIXE (HR-PIXE) spectroscopy in the tender X-ray range performed in our laboratory with our home-built tender X-ray emission spectrometer. Some general properties of high energy resolution PIXE spectroscopy in the tender X-ray range are presented followed by an example of sulfur speciation in biological tissue illustrating the capabilities as well as limitations of HR-PIXE method used for chemical speciation in the tender X-ray range.

Development of an X-ray fluorescence holographic measurement system for protein crystals

NASA Astrophysics Data System (ADS)

Sato-Tomita, Ayana; Shibayama, Naoya; Happo, Naohisa; Kimura, Koji; Okabe, Takahiro; Matsushita, Tomohiro; Park, Sam-Yong; Sasaki, Yuji C.; Hayashi, Kouichi

2016-06-01

Experimental procedure and setup for obtaining X-ray fluorescence hologram of crystalline metalloprotein samples are described. Human hemoglobin, an α2β2 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 mm3) 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.

X-ray Diffraction from Membrane Protein Nanocrystals

PubMed Central

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

2011-01-01

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

X-ray Scintillation in Lead Halide Perovskite Crystals

PubMed Central

Birowosuto, M. D.; Cortecchia, D.; Drozdowski, W.; Brylew, K.; Lachmanski, W.; Bruno, A.; Soci, C.

2016-01-01

Current technologies for X-ray detection rely on scintillation from expensive inorganic crystals grown at high-temperature, which so far has hindered the development of large-area scintillator arrays. Thanks to the presence of heavy atoms, solution-grown hybrid lead halide perovskite single crystals exhibit short X-ray absorption length and excellent detection efficiency. Here we compare X-ray scintillator characteristics of three-dimensional (3D) MAPbI3 and MAPbBr3 and two-dimensional (2D) (EDBE)PbCl4 hybrid perovskite crystals. X-ray excited thermoluminescence measurements indicate the absence of deep traps and a very small density of shallow trap states, which lessens after-glow effects. All perovskite single crystals exhibit high X-ray excited luminescence yields of >120,000 photons/MeV at low temperature. Although thermal quenching is significant at room temperature, the large exciton binding energy of 2D (EDBE)PbCl4 significantly reduces thermal effects compared to 3D perovskites, and moderate light yield of 9,000 photons/MeV can be achieved even at room temperature. This highlights the potential of 2D metal halide perovskites for large-area and low-cost scintillator devices for medical, security and scientific applications. PMID:27849019

Towards protein-crystal centering using second-harmonic generation (SHG) microscopy

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

Kissick, David J.; Dettmar, Christopher M.; Becker, Michael

2013-05-01

The potential of second-harmonic generation (SHG) microscopy for automated crystal centering to guide synchrotron X-ray diffraction of protein crystals has been explored. The potential of second-harmonic generation (SHG) microscopy for automated crystal centering to guide synchrotron X-ray diffraction of protein crystals was explored. These studies included (i) comparison of microcrystal positions in cryoloops as determined by SHG imaging and by X-ray diffraction rastering and (ii) X-ray structure determinations of selected proteins to investigate the potential for laser-induced damage from SHG imaging. In studies using β{sub 2} adrenergic receptor membrane-protein crystals prepared in lipidic mesophase, the crystal locations identified by SHGmore » images obtained in transmission mode were found to correlate well with the crystal locations identified by raster scanning using an X-ray minibeam. SHG imaging was found to provide about 2 µm spatial resolution and shorter image-acquisition times. The general insensitivity of SHG images to optical scatter enabled the reliable identification of microcrystals within opaque cryocooled lipidic mesophases that were not identified by conventional bright-field imaging. The potential impact of extended exposure of protein crystals to five times a typical imaging dose from an ultrafast laser source was also assessed. Measurements of myoglobin and thaumatin crystals resulted in no statistically significant differences between structures obtained from diffraction data acquired from exposed and unexposed regions of single crystals. Practical constraints for integrating SHG imaging into an active beamline for routine automated crystal centering are discussed.« less

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

PubMed

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

2018-04-24

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

Crystal doping aided by rapid expansion of supercritical solutions.

PubMed

Vemavarapu, Chandra; Mollan, Matthew J; Needham, Thomas E

2002-01-01

The purpose of this study was to test the utility of rapid expansion of supercritical solution (RESS) based cocrystallizations in inducing polymorph conversion and crystal disruption of chlorpropamide (CPD). CPD crystals were recrystallized by the RESS process utilizing supercritical carbon dioxide as the solvent. The supercritical region investigated for solute extraction ranged from 45 to 100 degrees C and 2000 to 8000 psi. While pure solute recrystallization formed stage I of these studies, stage II involved recrystallization of CPD in the presence of urea (model impurity). The composition, morphology, and crystallinity of the particles thus produced were characterized utilizing techniques such as microscopy, thermal analysis, x-ray powder diffractometry, and high-performance liquid chromatography. Also, comparative evaluation between RESS and evaporative crystallization from liquid solvents was performed. RESS recrystallizations of commercially available CPD (form A) resulted in polymorph conversion to metastable forms C and V, depending on the temperature and pressure of the recrystallizing solvent. Cocrystallization studies revealed the formation of eutectic mixtures and solid solutions of CPD + urea. Formation of the solid solutions resulted in the crystal disruption of CPD and subsequent amorphous conversion at urea levels higher than 40% wt/wt. Consistent with these results were the reductions in melting point (up to 9 degrees C) and in the DeltaH(f) values of CPD (up to 50%). Scanning electron microscopy revealed a particle size reduction of up to an order of magnitude upon RESS processing. Unlike RESS, recrystallizations from liquid organic solvents lacked the ability to affect polymorphic conversions. Also, the incorporation of urea into the lattice of CPD was found to be inadequate. In providing the ability to control both the particle and crystal morphologies of active pharmaceutical ingredients, RESS proved potentially advantageous to crystal engineering. Rapid crystallization kinetics were found vital in making RESS-based doping superior to conventional solvent-based cocrystallizations.

Crystallization and demineralization phenomena in washed-rind cheese.

PubMed

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/).

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

PubMed

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

2014-10-01

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

Crystallization and preliminary X-ray analysis of copper amine oxidase from Escherichia coli K-12.

PubMed

Roh, J H; Suzuki, H; Kumagai, H; Yamashita, M; Azakami, H; Murooka, Y; Mikami, B

1994-05-13

Copper-containing monoamine oxidase (MAO) from Escherichia coli was overproduced in the periplasmic space by expression of the cloned gene. The purified MAO has been crystallized by means of the hanging drop technique using sodium citrate as a precipitant. The crystals belong to the orthorhombic system, space group P2(1)2(1)2(1), with unit cell dimensions of a = 136.1 A, b = 168.4 A and c = 81.6 A. The asymmetric unit contains one molecule of MAO, with a crystal volume per protein mass (Vm) of 2.88 A3/Da and a solvent content of 58% by volume. The crystals diffract X-rays to a resolution limit of at least 2.7 A and are resistant to X-ray radiation damage. They appear to be suitable for X-ray structure analysis.

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

PubMed

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

2016-01-01

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

Performance of the x-ray free-electron laser oscillator with crystal cavity

NASA Astrophysics Data System (ADS)

Lindberg, R. R.; Kim, K.-J.; Shvyd'Ko, Yu.; Fawley, W. M.

2011-01-01

Simulations of the x-ray free-electron laser (FEL) oscillator are presented that include the frequency-dependent Bragg crystal reflectivity and the transverse diffraction and focusing using the two-dimensional FEL code GINGER. A review of the physics of Bragg crystal reflectors and the x-ray FEL oscillator is made, followed by a discussion of its numerical implementation in GINGER. The simulation results for a two-crystal cavity and realistic FEL parameters indicate ˜109 photons in a nearly Fourier-limited, ps pulse. Compressing the electron beam to 100 A and 100 fs results in comparable x-ray characteristics for relaxed beam emittance, energy spread, and/or undulator parameters, albeit in a larger radiation bandwidth. Finally, preliminary simulation results indicate that the four-crystal FEL cavity can be tuned in energy over a range of a few percent.

Improvement of graphite crystal analyzer for light elements on X-ray fluorescence holography measurement

NASA Astrophysics Data System (ADS)

Happo, Naohisa; Hada, Takuma; Kubota, Atsushi; Ebisu, Yoshihiro; Hosokawa, Shinya; Kimura, Koji; Tajiri, Hiroo; Matsushita, Tomohiro; Hayashi, Kouichi

2018-05-01

Using a graphite crystal analyzer, focused monochromatic fluorescent X-rays can be obtained on an X-ray fluorescence holography (XFH) measurement. To measure the holograms of elements lighter than Ti, we improved a cylindrical-type crystal analyzer and constructed a small C-shaped analyzer. Using the constructed C-shaped analyzer, a Ca Kα hologram of a fluorite single crystal was obtained, from which we reconstructed a clear atomic image. The XFH measurements for the K, Ca, and Sc elements become possible using the presently constructed analyzer.

Data reduction and analysis for the graphite crystal X-ray spectrometer and polarimeter experiment flown aboard OSO-8 spacecraft

NASA Technical Reports Server (NTRS)

Novick, R.

1980-01-01

The documentation and software programs developed for the reception, initial processing (quickbook), and production analysis of data obtained by solar X-ray spectroscopy, stellar spectroscopy, and X-ray polarimetry experiments on OSO-8 are listed. The effectiveness and sensitivity of the Bragg crystal scattering instruments used are assessed. The polarization data polarimetric data obtained shows that some X-ray sources are polarized and that a larger polarimeter of this type is required to perform the measurements necessary to fully understand the physics of X-ray sources. The scanning Bragg crystal spectrometer was ideally suited for studying rapidly changing solar conditions. Observations of the Crab Nebula and pulsar, Cyg X-1, Cyg X-2, Cyg X-3, Sco X-1, Cen X-3, and Her X-1 are discussed as well as of 4U1656-53 and 4U1820-30. Evidence was obtained for iron line emission from Cyg X-3.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source

NASA Astrophysics Data System (ADS)

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source.

PubMed

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystals

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

Haugh, M. J., E-mail: haughmj@nv.doe.gov; Jacoby, K. D.; Wu, M.

2014-11-15

This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals thatmore » we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.« less

Calculation of x-ray scattering patterns from nanocrystals at high x-ray intensity

PubMed Central

Abdullah, Malik Muhammad; Jurek, Zoltan; Son, Sang-Kil; Santra, Robin

2016-01-01

We present a generalized method to describe the x-ray scattering intensity of the Bragg spots in a diffraction pattern from nanocrystals exposed to intense x-ray pulses. Our method involves the subdivision of a crystal into smaller units. In order to calculate the dynamics within every unit, we employ a Monte-Carlo-molecular dynamics-ab-initio hybrid framework using real space periodic boundary conditions. By combining all the units, we simulate the diffraction pattern of a crystal larger than the transverse x-ray beam profile, a situation commonly encountered in femtosecond nanocrystallography experiments with focused x-ray free-electron laser radiation. Radiation damage is not spatially uniform and depends on the fluence associated with each specific region inside the crystal. To investigate the effects of uniform and non-uniform fluence distribution, we have used two different spatial beam profiles, Gaussian and flattop. PMID:27478859

Combining X-ray and neutron crystallography with spectroscopy.

PubMed

Kwon, Hanna; Smith, Oliver; Raven, Emma Lloyd; Moody, Peter C E

2017-02-01

X-ray protein crystallography has, through the determination of the three-dimensional structures of enzymes and their complexes, been essential to the understanding of biological chemistry. However, as X-rays are scattered by electrons, the technique has difficulty locating the presence and position of H atoms (and cannot locate H + ions), knowledge of which is often crucially important for the understanding of enzyme mechanism. Furthermore, X-ray irradiation, through photoelectronic effects, will perturb the redox state in the crystal. By using single-crystal spectrophotometry, reactions taking place in the crystal can be monitored, either to trap intermediates or follow photoreduction during X-ray data collection. By using neutron crystallography, the positions of H atoms can be located, as it is the nuclei rather than the electrons that scatter neutrons, and the scattering length is not determined by the atomic number. Combining the two techniques allows much greater insight into both reaction mechanism and X-ray-induced photoreduction.

Two-dimensional single crystal diamond refractive x-ray lens

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

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

2016-07-27

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

Preparation, characterization and millimetre wave attenuation performance of carbon fibers coated with nickel-wolfram-phosphorus and nickel-cobalt-wolfram- phosphorus

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

Ye, Mingquan; Li, Zhitao; Wang, Chen

2016-04-15

Highlights: • SEM, XRD, EDS and MMW attenuation performances of alloys coated CFs were studied. • Resistivity and P content in alloys were main factors on MMW attenuation property. • The weight gain of coated CFs has effects on the MMW attenuation performance. - Abstract: Carbon fibers (CFs) coated with Ni–X–P (X = W, Co–W or none) alloys were prepared by electroless plating. The morphology, crystal structure, and element composition of alloy-coated CFs were characterized by scanning electron microscopy, X-ray diffractometry, energy-dispersive spectrometry and microwave attenuation. The results showed that CFs were coated with a layer of alloy particles. Pmore » content in Ni–Co–W–P or Ni–W–P alloys was lower than that in Ni–P alloy, and coating alloy Ni–P was amorphous. After W or Co introduction, coating alloys exhibited crystal characteristics. MMW-attenuation performance analysis showed that the 3 mm wave attenuation performance of CFs/Ni–Co–W–P, CFs/Ni–W–P and CFs/Ni–P increased by 7.27 dBm, 4.88 dBm and 3.55 dBm, and the 8 mm wave attenuation effects increased by 11.61 dBm, 6.11 dBm, and 4.06 dBm respectively, compared with those of CFs. MMW-attenuation performance is attributable to the sample bulk resistivity and P content in the alloy. Moreover, an optimal weight gain value existed for the MMW-attenuation performance of alloy-coated CFs.« less

Sagittal focusing Laue monochromator

DOEpatents

Zhong,; Zhong, Hanson [Stony Brook, NY; Jonathan, Hastings [Wading River, NY; Jerome, Kao [Stanford, CA; Chi-Chang, Lenhard [Setauket, NY; Anthony, Siddons [Medford, NY; David Peter, Zhong [Cutchogue, NY; Hui, [Coram, NY

2009-03-24

An x-ray focusing device generally includes a slide pivotable about a pivot point defined at a forward end thereof, a rail unit fixed with respect to the pivotable slide, a forward crystal for focusing x-rays disposed at the forward end of the pivotable slide and a rearward crystal for focusing x-rays movably coupled to the pivotable slide and the fixed rail unit at a distance rearward from the forward crystal. The forward and rearward crystals define reciprocal angles of incidence with respect to the pivot point, wherein pivoting of the slide about the pivot point changes the incidence angles of the forward and rearward crystals while simultaneously changing the distance between the forward and rearward crystals.

Investigating the Effect of Impurities on Macromolecule Crystal Growth in Microgravity

NASA Technical Reports Server (NTRS)

Snell, Edward H.; Judge, Russell A.; Crawford, Lisa; Forsythe, Elizabeth L.; Pusey, Marc L.; Sportiello, Michael; Todd, Paul; Bellamy, Henry; Lovelace, Jeff; Cassanto, John M.;

Solid state structural investigations of the bis(chalcone) compound with single crystal X-ray crystallography, DFT, gamma-ray spectroscopy and chemical spectroscopy methods

NASA Astrophysics Data System (ADS)

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.

Improving Beamline X-ray Optics by Analyzing the Damage to Crystallographic Structure

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

Zientek, John; Maj, Jozef; Navrotski, Gary

2015-01-02

The mission of the X-ray Characterization Laboratory in the X-ray Science Division (XSD) at the Advanced Photon Source (APS) is to support both the users and the Optics Fabrication Facility that produces high performance optics for synchrotron X-ray beamlines. The Topography Test Unit (TTU) in the X-ray Lab has been successfully used to characterize diffracting crystals and test monochromators by quantifying residual surface stresses. This topographic method has also been adapted for testing standard X-ray mirrors, characterizing concave crystal optics and in principle, can be used to visualize residual stresses on any optic made from single crystalline material. The TTUmore » has been instrumental in quantitatively determining crystal mounting stresses which are mechanically induced by positioning, holding, and cooling fixtures. It is this quantitative aspect that makes topography so useful since the requirements and responses for crystal optics and X-ray mirrors are quite different. In the case of monochromator crystals, even small residual or induced stresses, on the order of tens of kPa, can cause detrimental distortions to the perfect crystal rocking curves. Mirrors, on the other hand, are much less sensitive to induced stresses where stresses that are an order of magnitude greater can be tolerated. This is due to the fact that the surface rather than the lattice-spacing determines a mirror’s performance. For the highly sensitive crystal optics, it is essential to measure the in-situ rocking curves using topographs as mounting fixtures are adjusted. In this way, high heat-load monochromator crystals can be successfully mounted with minimum stress. Topographical analysis has been shown to be a highly effective method to visualize and quantify the distribution of stresses, to help identify methods that mitigate stresses, and most notably to improve diffractive crystal optic rocking curves.« less

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

DOE PAGES

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

2016-01-01

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

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

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

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

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

Bulk vertical micromachining of single-crystal sapphire using inductively coupled plasma etching for x-ray resonant cavities

NASA Astrophysics Data System (ADS)

Chen, P.-C.; Lin, P.-T.; Mikolas, D. G.; Tsai, Y.-W.; Wang, Y.-L.; Fu, C.-C.; Chang, S.-L.

2015-01-01

To provide coherent x-ray sources for probing the dynamic structures of solid or liquid biological substances on the picosecond timescale, a high-aspect-ratio x-ray resonator cavity etched from a single crystal substrate with a nearly vertical sidewall structure is required. Although high-aspect-ratio resonator cavities have been produced in silicon, they suffer from unwanted multiple beam effects. However, this problem can be avoided by using the reduced symmetry of single-crystal sapphire in which x-ray cavities may produce a highly monochromatic transmitted x-ray beam. In this study, we performed nominal 100 µm deep etching and vertical sidewall profiles in single crystal sapphire using inductively coupled plasma (ICP) etching. The large depth is required to intercept a useful fraction of a stopped-down x-ray beam, as well as for beam clearance. An electroplated Ni hard mask was patterned using KMPR 1050 photoresist and contact lithography. The quality and performance of the x-ray cavity depended upon the uniformity of the cavity gap and therefore verticality of the fabricated vertical sidewall. To our knowledge, this is the first report of such deep, vertical etching of single-crystal sapphire. A gas mixture of Cl2/BCl3/Ar was used to etch the sapphire with process variables including BCl3 flow ratio and bias power. By etching for 540 min under optimal conditions, we obtained an x-ray resonant cavity with a depth of 95 µm, width of ~30 µm, gap of ~115 µm and sidewall profile internal angle of 89.5°. The results show that the etching parameters affected the quality of the vertical sidewall, which is essential for good x-ray resonant cavities.

X-ray tests of a two-dimensional stigmatic imaging scheme with variable magnifications

DOE PAGES

Lu, J.; Bitter, M.; Hill, K. W.; ...

2014-07-22

A two-dimensional stigmatic x-ray imaging scheme, consisting of two spherically bent crystals, one concave and one convex, was recently proposed [M. Bitter et al., Rev. Sci. Instrum. 83, 10E527 (2012)]. We report that the Bragg angles and the radii of curvature of the two crystals of this imaging scheme are matched to eliminate the astigmatism and to satisfy the Bragg condition across both crystal surfaces for a given x-ray energy. In this paper, we consider more general configurations of this imaging scheme, which allow us to vary the magnification for a given pair of crystals and x-ray energy. The stigmaticmore » imaging scheme has been validated for the first time by imaging x-rays generated by a micro-focus x-ray source with source size of 8.4 μm validated by knife-edge measurements. Results are presented from imaging the tungsten Lα1 emission at 8.3976 keV, using a convex Si-422 crystal and a concave Si-533 crystal with 2d-spacings of 2.21707 Å and 1.65635 Å and radii of curvature of 500 ± 1 mm and 823 ± 1 mm, respectively, showing a spatial resolution of 54.9 μm. Finally, this imaging scheme is expected to be of interest for the two-dimensional imaging of laser produced plasmas.« less

Crystals and collimators for X-ray spectrometry. [Bragg reflection properties and design for astronomical applications

NASA Technical Reports Server (NTRS)

Mckenzie, D. L.; Landecker, P. B.; Underwood, J. H.

1976-01-01

Results of the measurement of Bragg reflection properties of crystals suitable for use in X-ray astronomy are presented. Measurements with a double crystal spectrometer were performed on rubidium acid phthalate and thallium acid phthalate to yield values of the integrated reflectivity and diffraction width in the range 8-18 A, and measurements of integrated reflectivity were also performed on ammonium dihydrogen phosphate. The theory and design of an arc-minute range multigrid collimator to be flown on a rocket for solar X-ray studies are also described, along with a method for determining the collimator's X-ray axis.

Imaging crystal/spectral line search

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

Koch, J.A.

1998-02-16

The following table is a compilation of chance coincidences between x- ray line wavelengths and crystal planes which will reflect those wavelengths near normal incidence. The motivation is to explore the possibilities for expanding the range of choices for near normal incidence x-ray crystal imaging.

Measuring the X-ray Resolving Power of Bent Potassium Acid Phthalate Diffraction Crystals

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

Haugh, M. J.; Wu, M.; Jacoby, K. D.

2014-11-01

This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals thatmore » we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories (SNL) in Albuquerque, NM. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a dual goniometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.« less

Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystalsa)

NASA Astrophysics Data System (ADS)

Haugh, M. J.; Wu, M.; Jacoby, K. D.; Loisel, G. P.

2014-11-01

This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

Sagittal focusing of synchrotron radiation X-rays using a winged crystal

PubMed Central

Nisawa, A.; Yoneda, Y.; Ueno, G.; Murakami, H.; Okajima, Y.; Yamamoto, K.; Senba, Y.; Uesugi, K.; Tanaka, Y.; Yamamoto, M.; Goto, S.; Ishikawa, T.

2013-01-01

A Si(111) winged crystal has been designed to minimize anticlastic bending and improve sagittal focusing efficiency. The crystal was thin with wide stiffening wings. The length-to-width ratio of the crystal was optimized by finite element analysis, and the optimal value was larger than the ‘golden value’. The analysis showed that the slope error owing to anticlastic bending is less than the Darwin width. The X-rays were focused two-dimensionally using the crystal and a tangentially bent mirror. The observed profiles of the focal spot agreed well with the results of a ray-tracing calculation in the energy range from 8 to 17.5 keV. X-ray diffraction measurements with a high signal-to-noise ratio using this focusing system were demonstrated for a small protein crystal. PMID:23412477

Quantitation of polymorphic impurity in entecavir polymorphic mixtures using powder X-ray diffractometry and Raman spectroscopy.

PubMed

Kang, Yanlei; Shao, Zhanying; Wang, Qiang; Hu, Xiurong; Yu, Dongdong

2018-05-26

Entecavir was used for the treatment of chronic hepatitis B through inhibiting hepatitis B virus. The anhydrous form of entecavir (ENT-A) often appeared as impurity polymorph in the manufacturing process of entecavir monohydrate (ENT-H) such as granulation, drying and compression. Since different crystal forms might affect drug bioavailability and therapeutic effect, it was vital to control the ENT-A content of the drug product. The work aimed to develop useful methods to assess ENT-A weight percentage in ENT-H. Powder X-ray diffractometry (PXRD) and Raman spectrometric methods were applied. Binary mixtures with different ratios of pure ENT-H and pure ENT-A were scanned using PXRD and Raman to obtain spectra. Then peak heights and peak areas versus weight percentage were used to construct calibration curves. The best linear regression analysis data for PXRD and Raman method were found to be R 2  = 0.9923 and R 2  = 0.9953, in the weight ratio range of 2.1-20.2% w/w% of ENT-A in binary mixtures. Limit of detection (LOD) of ENT-A was 0.38% and limit of quantitation (LOQ) was 1.15% for PXRD method. LOD and LOQ for Raman method were 0.48% and 1.16%. The results showed that PXRD and Raman methods: both were precise and accurate, and could be used for measurement of ENT-A content in the selected weight percentage range. Partial least squares (PLS) algorithm with four data pre-processing methods: including multiplicative scatter correlation (MSC), standard normal variate (SNV), first and second derivatives were applied and evaluated using prediction errors. The best performance of PLS was R 2  = 0.9958 with RMSEC (0.44%) and RMSEP (0.65%). Multivariate analysis for Raman spectra showed similar good results with univariate analysis, and would be an advantageous method when there were overlapped peaks in the spectra. In summary, the proposed PXRD and Raman method could be developed for the quality control of ENT-H. And Raman was a more promising method in industrial practice due to its slightly better precision, accuracy and time-saving advantage. Copyright © 2018 Elsevier B.V. All rights reserved.

Studies of x-ray localization and thickness dependence in atomic-scale elemental mapping by STEM energy-dispersive x-ray spectroscopy using single-frame scanning method

DOE PAGES

Lu, Ping; Moya, Jaime M.; Yuan, Renliang; ...

2018-03-01

The delocalization of x-ray signals limits the spatial resolution in atomic-scale elemental mapping by scanning transmission electron microscopy (STEM) using energy-dispersive x-ray spectroscopy (EDS). In this study, using a SrTiO 3 [001] single crystal, we show that the x-ray localization to atomic columns is strongly dependent on crystal thickness, and a thin crystal is critical for improving the spatial resolution in atomic-scale EDS mapping. A single-frame scanning technique is used in this study instead of the multiple-frame technique to avoid peak broadening due to tracking error. The strong thickness dependence is realized by measuring the full width at half maximamore » (FWHM) as well as the peak-to-valley (P/V) ratio of the EDS profiles for Ti K and Sr K+L, obtained at several crystal thicknesses. A FWHM of about 0.16 nm and a P/V ratio of greater than 7.0 are obtained for Ti K for a crystal thickness of less than 20 nm. In conclusion, with increasing crystal thickness, the FWHM and P/V ratio increases and decreases, respectively, indicating the advantage of using a thin crystal for high-resolution EDS mapping.« less

Studies of x-ray localization and thickness dependence in atomic-scale elemental mapping by STEM energy-dispersive x-ray spectroscopy using single-frame scanning method

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

Lu, Ping; Moya, Jaime M.; Yuan, Renliang

The delocalization of x-ray signals limits the spatial resolution in atomic-scale elemental mapping by scanning transmission electron microscopy (STEM) using energy-dispersive x-ray spectroscopy (EDS). In this study, using a SrTiO 3 [001] single crystal, we show that the x-ray localization to atomic columns is strongly dependent on crystal thickness, and a thin crystal is critical for improving the spatial resolution in atomic-scale EDS mapping. A single-frame scanning technique is used in this study instead of the multiple-frame technique to avoid peak broadening due to tracking error. The strong thickness dependence is realized by measuring the full width at half maximamore » (FWHM) as well as the peak-to-valley (P/V) ratio of the EDS profiles for Ti K and Sr K+L, obtained at several crystal thicknesses. A FWHM of about 0.16 nm and a P/V ratio of greater than 7.0 are obtained for Ti K for a crystal thickness of less than 20 nm. In conclusion, with increasing crystal thickness, the FWHM and P/V ratio increases and decreases, respectively, indicating the advantage of using a thin crystal for high-resolution EDS mapping.« less

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

Schollmeier, Marius S.; Loisel, Guillaume P.

Spherical-crystal microscopes are used as high-resolution imaging devices for monochromatic x-ray radiography or for imaging the source itself. Crystals and Miller indices (hkl) have to be matched such that the resulting lattice spacing d is close to half the spectral wavelength used for imaging, to fulfill the Bragg equation with a Bragg angle near 90° which reduces astigmatism. Only a few suitable crystal and spectral-line combinations have been identified for applications in the literature, suggesting that x-ray imaging using spherical crystals is constrained to a few chance matches. In this paper, after performing a systematic, automated search over more thanmore » 9 × 10 6 possible combinations for x-ray energies between 1 and 25 keV, for six crystals with arbitrary Miller-index combinations hkl between 0 and 20, we show that a matching, efficient crystal and spectral-line pair can be found for almost every He α or K α x-ray source for the elements Ne to Sn. Finally, using the data presented here it should be possible to find a suitable imaging combination using an x-ray source that is specifically selected for a particular purpose, instead of relying on the limited number of existing crystal imaging systems that have been identified to date.« less

Studies of x-ray localization and thickness dependence in atomic-scale elemental mapping by STEM energy-dispersive x-ray spectroscopy using single-frame scanning method.

PubMed

Lu, Ping; Moya, Jaime M; Yuan, Renliang; Zuo, Jian Min

2018-03-01

The delocalization of x-ray signals limits the spatial resolution in atomic-scale elemental mapping by scanning transmission electron microscopy (STEM) using energy-dispersive x-ray spectroscopy (EDS). In this study, using a SrTiO 3 [001] single crystal, we show that the x-ray localization to atomic columns is strongly dependent on crystal thickness, and a thin crystal is critical for improving the spatial resolution in atomic-scale EDS mapping. A single-frame scanning technique is used in this study instead of the multiple-frame technique to avoid peak broadening due to tracking error. The strong thickness dependence is realized by measuring the full width at half maxima (FWHM) as well as the peak-to-valley (P/V) ratio of the EDS profiles for Ti K and Sr K + L, obtained at several crystal thicknesses. A FWHM of about 0.16 nm and a P/V ratio of greater than 7.0 are obtained for Ti K for a crystal thickness of less than 20 nm. With increasing crystal thickness, the FWHM and P/V ratio increases and decreases, respectively, indicating the advantage of using a thin crystal for high-resolution EDS mapping. Published by Elsevier B.V.

Sensitive X-ray detectors made of methylammonium lead tribromide perovskite single crystals

NASA Astrophysics Data System (ADS)

Wei, Haotong; Fang, Yanjun; Mulligan, Padhraic; Chuirazzi, William; Fang, Hong-Hua; Wang, Congcong; Ecker, Benjamin R.; Gao, Yongli; Loi, Maria Antonietta; Cao, Lei; Huang, Jinsong

2016-05-01

The large mobilities and carrier lifetimes of hybrid perovskite single crystals and the high atomic numbers of Pb, I and Br make them ideal for X-ray and gamma-ray detection. Here, we report a sensitive X-ray detector made of methylammonium lead bromide perovskite single crystals. A record-high mobility-lifetime product of 1.2 × 10-2 cm2 V-1 and an extremely small surface charge recombination velocity of 64 cm s-1 are realized by reducing the bulk defects and passivating surface traps. Single-crystal devices with a thickness of 2-3 mm show 16.4% detection efficiency at near zero bias under irradiation with continuum X-ray energy up to 50 keV. The lowest detectable X-ray dose rate is 0.5 μGyair s-1 with a sensitivity of 80 μC Gy-1air cm-2, which is four times higher than the sensitivity achieved with α-Se X-ray detectors. This allows the radiation dose applied to a human body to be reduced for many medical and security check applications.

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

PubMed

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

2016-02-01

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

Synthesis and characterization of zeolites prepared from industrial fly ash.

PubMed

Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

2014-09-01

In this paper, we present the possibility of using fly ash to produce synthetic zeolites. The synthesis class F fly ash from the Stalowa Wola SA heat and power plant was subjected to 24 h hydrothermal reaction with sodium hydroxide. Depending on the reaction conditions, three types of synthetic zeolites were formed: Na-X (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 75 °C), Na-P1 (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 95 °C), and sodalite (20 g fly ash, 0.8 dm(3) of 5 mol · dm(-3) NaOH + 0.4 dm(3) of 3 mol · dm(-3) NaCl, 95 °C). As synthesized materials were characterized to obtain mineral composition (X-ray diffractometry, Scanning electron microscopy-energy dispersive spectrometry), adsorption properties (Brunauer-Emmett-Teller surface area, N2 isotherm adsorption/desorption), and ion exchange capacity. The most effective reaction for zeolite preparation was when sodalite was formed and the quantitative content of zeolite from X-ray diffractometry was 90 wt%, compared with 70 wt% for the Na-X and 75 wt% for the Na-P1. Residues from each synthesis reaction were the following: mullite, quartz, and the remains of amorphous aluminosilicate glass. The best zeolitic material as characterized by highest specific surface area was Na-X at almost 166 m(2) · g(-1), while for the Na-P1 and sodalite it was 71 and 33 m(2) · g(-1), respectively. The ion exchange capacity decreased in the following order: Na-X at 1.8 meq · g(-1), Na-P1 at 0.72 meq · g(-1), and sodalite at 0.56 meq · g(-1). The resulting zeolites are competitive for commercially available materials and are used as ion exchangers in industrial wastewater and soil decontamination.

X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

NASA Astrophysics Data System (ADS)

Zhou, X. Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A.; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W.; Suino-Powell, Kelly M.; Boutet, Sébastien; Williams, Garth J.; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N.; Spence, John C. H.; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C.; Cherezov, Vadim; Melcher, Karsten; Xu, H. Eric

2016-04-01

Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.

Three-energy focusing Laue monochromator for the diamond light source x-ray pair distribution function beamline I15-1

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

Sutter, John P., E-mail: john.sutter@diamond.ac.uk; Chater, Philip A.; Hillman, Michael R.

2016-07-27

The I15-1 beamline, the new side station to I15 at the Diamond Light Source, will be dedicated to the collection of atomic pair distribution function data. A Laue monochromator will be used consisting of three silicon crystals diffracting X-rays at a common Bragg angle of 2.83°. The crystals use the (1 1 1), (2 2 0), and (3 1 1) planes to select 40, 65, and 76 keV X-rays, respectively, and will be bent meridionally to horizontally focus the selected X-rays onto the sample. All crystals will be cut to the same optimized asymmetry angle in order to eliminate imagemore » broadening from the crystal thickness. Finite element calculations show that the thermal distortion of the crystals will affect the image size and bandpass.« less

Monitoring the recrystallisation of amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering.

PubMed

Palomäki, Emmi; Ahvenainen, Patrik; Ehlers, Henrik; Svedström, Kirsi; Huotari, Simo; Yliruusi, Jouko

2016-07-11

In this paper we present a fast model system for monitoring the recrystallization of quench-cooled amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering. The use of these two methods enables comparison between surface and bulk crystallization. Non-ordered mesoporous silica micro-particles were added to the system in order to alter the rate of crystallization of the amorphous xylitol. Raman measurements showed that adding silica to the system increased the rate of surface crystallization, while X-ray measurements showed that the rate of bulk crystallization decreased. Using this model system it is possible to measure fast changes, which occur in minutes or within a few hours. Raman-spectroscopy and wide-angle X-ray scattering were found to be complementary techniques when assessing surface and bulk crystallization of amorphous xylitol. Copyright © 2016 Elsevier B.V. All rights reserved.

X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex.

PubMed

Zhou, X Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W; Suino-Powell, Kelly M; Boutet, Sébastien; Williams, Garth J; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N; Spence, John C H; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C; Cherezov, Vadim; Melcher, Karsten; Xu, H Eric

2016-04-12

Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.

X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

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

Zhou, X. Edward; Gao, Xiang; Barty, Anton

Here, serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solvedmore » with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.« less

X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

PubMed Central

Zhou, X. Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A.; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W.; Suino-Powell, Kelly M.; Boutet, Sébastien; Williams, Garth J.; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N.; Spence, John C.H.; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C.; Cherezov, Vadim; Melcher, Karsten; Xu, H. Eric

2016-01-01

Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes. PMID:27070998

X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

DOE PAGES

Zhou, X. Edward; Gao, Xiang; Barty, Anton; ...

2016-04-12

Here, serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solvedmore » with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.« less

Development of an x-ray prism for analyzer based imaging systems

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

Bewer, Brian; Chapman, Dean

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP)more » was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.« less

Development of an x-ray prism for analyzer based imaging systems

NASA Astrophysics Data System (ADS)

Bewer, Brian; Chapman, Dean

2010-08-01

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP) was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.

Development of an x-ray prism for analyzer based imaging systems.

PubMed

Bewer, Brian; Chapman, Dean

2010-08-01

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP) was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.

Crystallization and preliminary X-ray diffraction analysis of a chitin-binding domain of hyperthermophilic chitinase from Pyrococcus furiosus

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

Nakamura, Tsutomu; Ishikawa, Kazuhiko; Hagihara, Yoshihisa

The expression, purification and preliminary X-ray diffraction studies of a chitin-binding domain of the chitinase from P. furiosus are reported. The crystallization and preliminary X-ray diffraction analysis of the chitin-binding domain of chitinase from a hyperthermophilic archaeon, Pyrococcus furiosus, are reported. The recombinant protein was prepared using an Escherichia coli overexpression system and was crystallized by the hanging-drop vapour-diffusion method. An X-ray diffraction data set was collected to 1.70 Å resolution. The crystal belonged to space group P4{sub 3}2{sub 1}2 or P4{sub 1}2{sub 1}2. The unit-cell parameters were determined to be a = b = 48.8, c = 85.0 Å.

Luminescence and Scintillation Properties of Czochralski Grown LYGBO Crystals

NASA Astrophysics Data System (ADS)

Fawad, U.; Kim, Hong Joo; Park, H.; Kim, Sunghwan; Khan, Sajid

2016-06-01

Mixed crystals Li6YxGd1-x(BO3)3:Ce3+ (LYGBO) (where, x = 0.0, 0.2, 0.5, 0.8, 1.0) are grown by using Czochralski method with different proportions of Li6Y(BO3)3 and Li6Gd(BO3)3. All crystals are doped with 3 mole% optimized concentrations of Ce3+ ions. The grown crystals are 20-70 mm in length and 5-10 mm in diameter. Detailed sintering and crystal growth procedure is presented in this study. The required phase of the grown crystals is confirmed by powder X-ray diffraction (XRD) analysis. Ultraviolet (UV) photoluminescence and X-ray induced luminescence of the grown crystals at room temperature are measured. Various scintillation properties such as energy resolution, light yield, α/β ratio and fluorescence decay time under the excitation by 137Cs γ-ray and 241Am particles are also presented.

Energy dispersive X-ray fluorescence spectroscopy/Monte Carlo simulation approach for the non-destructive analysis of corrosion patina-bearing alloys in archaeological bronzes: The case of the bowl from the Fareleira 3 site (Vidigueira, South Portugal)

NASA Astrophysics Data System (ADS)

Bottaini, C.; Mirão, J.; Figuereido, M.; Candeias, A.; Brunetti, A.; Schiavon, N.

2015-01-01

Energy dispersive X-ray fluorescence (EDXRF) is a well-known technique for non-destructive and in situ analysis of archaeological artifacts both in terms of the qualitative and quantitative elemental composition because of its rapidity and non-destructiveness. In this study EDXRF and realistic Monte Carlo simulation using the X-ray Monte Carlo (XRMC) code package have been combined to characterize a Cu-based bowl from the Iron Age burial from Fareleira 3 (Southern Portugal). The artifact displays a multilayered structure made up of three distinct layers: a) alloy substrate; b) green oxidized corrosion patina; and c) brownish carbonate soil-derived crust. To assess the reliability of Monte Carlo simulation in reproducing the composition of the bulk metal of the objects without recurring to potentially damaging patina's and crust's removal, portable EDXRF analysis was performed on cleaned and patina/crust coated areas of the artifact. Patina has been characterized by micro X-ray Diffractometry (μXRD) and Back-Scattered Scanning Electron Microscopy + Energy Dispersive Spectroscopy (BSEM + EDS). Results indicate that the EDXRF/Monte Carlo protocol is well suited when a two-layered model is considered, whereas in areas where the patina + crust surface coating is too thick, X-rays from the alloy substrate are not able to exit the sample.

X-ray crystal structure and small-angle X-ray scattering of sheep liver sorbitol dehydrogenase

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

Yennawar, Hemant; Møller, Magda; University of Copenhagen, DK-2100 Copenhagen

The X-ray crystal structure and a small-angle X-ray scattering solution structure of sheep liver sorbitol dehydrogenase have been determined. The details of the interactions that enable the tetramer scaffold to be the functional biological unit have been analyzed. The X-ray crystal structure of sheep liver sorbitol dehydrogenase (slSDH) has been determined using the crystal structure of human sorbitol dehydrogenase (hSDH) as a molecular-replacement model. slSDH crystallized in space group I222 with one monomer in the asymmetric unit. A conserved tetramer that superposes well with that seen in hSDH (despite belonging to a different space group) and obeying the 222 crystalmore » symmetry is seen in slSDH. An acetate molecule is bound in the active site, coordinating to the active-site zinc through a water molecule. Glycerol, a substrate of slSDH, also occupies the substrate-binding pocket together with the acetate designed by nature to fit large polyol substrates. The substrate-binding pocket is seen to be in close proximity to the tetramer interface, which explains the need for the structural integrity of the tetramer for enzyme activity. Small-angle X-ray scattering was also used to identify the quaternary structure of the tetramer of slSDH in solution.« less

Diamond x-ray optics: Transparent, resilient, high-resolution, and wavefront preserving

DOE PAGES

Shvyd’ko, Yuri; Blank, Vladimir; Terentyev, Sergey

2017-06-09

Diamond features a unique combination of outstanding physical properties perfect for numerous x-ray optics applications, where traditional materials such as silicon fail to perform. In the last two decades, impressive progress has been achieved in synthesizing diamond with high crystalline perfection, in manufacturing efficient, resilient, high-resolution, wavefront-preserving diamond optical components, and in implementing them in cutting-edge x-ray instruments. Diamond optics are essential for tailoring x-rays to the most challenging needs of x-ray research. Furthermore, they are becoming vital for the generation of fully coherent hard x-rays by seeded x-ray free-electron lasers. In this article, we review progress in manufacturing flawlessmore » diamond crystal components and their applications in diverse x-ray optical devices, such as x-ray monochromators, beam splitters, high-reflectance backscattering mirrors, lenses, phase plates, diffraction gratings, bent-crystal spectrographs, and windows.« less

Spectroellipsometric studies of sol-gel derived Sr0.6Ba0.4Nb2O6 films

NASA Astrophysics Data System (ADS)

Ho, Melanie M. T.; Tang, T. B.; Mak, C. L.; Pang, G. K. H.; Chan, K. Y.; Wong, K. H.

2006-10-01

Sr0.6Ba0.4Nb2O6 (SBN) films have been fabricated on (001)Si substrates by a sol-gel technique. The annealing process was carried out in air at various temperatures ranging from 200to700°C. Studies using x-ray diffractometry, high resolution transmission electron microscopy, and scanning electron microscopy showed that polycrystalline films, with a grain size of about 100nm, were obtained only for annealing temperatures ⩾600°C. The optical properties of these sol-gel derived SBN films were studied by spectroscopic ellipsometry (SE). In the analysis of the measured SE spectra, a triple-layer Lorentz model has been developed and used to deduce the optical properties of the SBN films. Our systematic SE measurements revealed that the refractive indices of the SBN films increase with the annealing temperature. This increase is more pronounced at around the crystallization temperature, i.e., between 500 and 600°C. The extinction coefficients of the films also exhibit a similar trend, showing a zero value for amorphous films and larger values for films annealed at above 600°C. Our results demonstrate that while crystallization helps to raise the refractive index of the film due to film densification, it also promotes scattering by grain boundary, resulting in a larger extinction coefficient.

Phenomenology of Polymorphism, III: p, TDiagram and Stability of Piracetam Polymorphs

NASA Astrophysics Data System (ADS)

Céolin, R.; Agafonov, V.; Louër, D.; Dzyabchenko, V. A.; Toscani, S.; Cense, J. M.

1996-02-01

The nootropic drug Piracetam is known to crystallize in three phases. In order to obtain their stability hierarchy from sublimation pressure inequalities, the drawing of a topologicalp,Tdiagram was attempted. For such a purpose and also for quality control, crystallographic and thermodynamic data were required. Powder X-ray diffractometry (XRD) and differential scanning calorimetry (DSC) were used. Molecular energy calculations were performed. Phase I melts at 426 K (ΔfusH(I) = +180 J·g-1). Phase II transforms into Phase I at 399 K (Δ(II→I)H= +24 J·g-1). Phase III transforms into phase I at 392 K (Δ(III→I)H= +28 J·g-1) or melts at 412 K (ΔfusH(III) = +210 J·g-1). Thep,Tdiagram shows that phase I is stable at higher temperature and phase II at lower temperature, like phase III, which is stable under high pressure. At room temperature, phase II is the more stable form, and phase I the less stable one. This agrees with the spontaneous I → II transformation observed at 298 K within a few hours, and with lattice energies, calculated previously. Molecular energy calculations and crystal structure comparison show how intermolecular hydrogen bonds and H-bonded dimers, in phases II and III, may stabilize conformations higher in energy than those of the isolated molecule and of phase I.

Enhancement of valve metal osteoconductivity by one-step hydrothermal treatment.

PubMed

Zuldesmi, Mansjur; Waki, Atsushi; Kuroda, Kensuke; Okido, Masazumi

2014-09-01

In this study, we produced super-hydrophilic surfaces of valve metals (Ti, Nb, Ta and Zr) by one-step hydrothermal treatment. Their surface characteristics and osteoconductivity using an in vivo test were then assessed. These data were compared with that of as-polished, as-anodized and both anodized+hydrothermally treated samples. Changes in surface chemistry, surface morphology and structure were investigated by X-ray photoelectron spectroscopy, scanning electron microscopy, and X-ray diffractometry. The results revealed that the water contact angles of valve metals were decreased by hydrothermal treatment and continued to reduce dramatically until lower than 10° after being immersed in phosphate buffered solution. By producing super-hydrophilic surfaces, the osteoconductivity of these hydrothermally treated valve metals was enhanced by up to 55%. Copyright © 2014 Elsevier B.V. All rights reserved.

Delaminating and restacking MgAl-layered double hydroxide monitored and characterized by a range of instrumental methods

NASA Astrophysics Data System (ADS)

Muráth, Szabolcs; Somosi, Zoltán; Tóth, Ildikó Y.; Tombácz, Etelka; Sipos, Pál; Pálinkó, István

2017-07-01

The delamination-restacking properties of MgAl-layered double hydroxide (MgAl-LDH) were studied in various solvents. The LDH samples were successfully delaminated in polar amides (formamide, N-methylformamide, N-methylacetamide). Usually, delamination was finalized by ultrasonic treatment. As rehydrating solutions, numerous Na-salts with single-, double- and triple-charged anions were used. Reconstruction was accomplished with anions of one or two negative charges, but triple-charged ones generally disrupted the rebuilding process, likely, because their salts with the metals of the LDH are very stable, and the thin layers can more readily transform to salts than the ordered materials. Samples and delamination-restacking processes were characterized by X-ray diffractometry (XRD), infrared spectroscopy (IR), dynamic light scattering (DLS), scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDX).

Carbon Coated α-Fe2O3 Photoanode Synthesized by a Facile Anodic Electrodeposition for Highly Efficient Water Oxidation

NASA Astrophysics Data System (ADS)

Zhang, Honglei; Li, Longzhu; Liu, Changhai; Wang, Wenchang; Liang, Penghua; Mitsuzak, Naotoshi; Chen, Zhidong

2018-05-01

This work provides a facile anodic electrodeposition method for synthesizing carbon coated α-Fe2O3 photoanode followed by annealing treatment with argon atmosphere. Compared with bare hematite photoanode, the carbon coated α-Fe2O3 photoanodes annealed at lower temperature (Fe2O3/C-L) and higher temperature (Fe2O3/C-H) have higher photocurrent density as 0.3 and 0.5 mA cm-2 (at 1.23 V vs. RHE), respectively. The excellent PEC performance is attributed to the synergistic reaction of carbon and vacancy oxygen. The morphology and properties of the sample were characterized with scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, UV-Vis spectra, X-ray diffractometry, X-ray photoelectron spectra, and photoelectrical measurements.

Thermal behavior of potato starch and water-vaporization behavior of its paste controlled with amino acid and peptide-rich food materials.

PubMed

Sakauchi, Satoshi; Hattori, Makoto; Yoshida, Tadashi; Yagishita, Takahiro; Ito, Koichi; Akemitsu, Shin-Ichi; Takahashi, Koji

2010-03-01

The particular effect of 4 kinds of amino acid and peptide-rich food material (APRM) containing different charged amino acid contents on the gelatinization and retrogradation behavior of potato starch granules and on the water-vaporization behavior was analyzed by differential scanning calorimetry, rapid viscoanalysis, x-ray diffractometry, thermal gravimetry-differential thermal analysis, and pulsed NMR. APRM with a high-charged amino acid content produced unique gelatinization and retrogradation behavior in terms of an elevated gelatinization temperature, reduced viscosity, higher setback, and lower retrograded starch melting enthalpy. The recovered x-ray diffraction intensity decreased with increasing charged amino acid content. APRM with high-charged amino acid content could provide an improved paste having easy vaporization of external water in the swollen starch granules due to the reduced swelling.

Laser formation of titanium nitride films as a result of Ti coating modification in a nitrogen atmosphere

NASA Astrophysics Data System (ADS)

Eskin, Sergei

1998-12-01

Laser treatment of the 303 and 416 stainless steels with Ti precoating was studied. CW CO2 and UV ArF excimer lasers were used. The TiN films were formed at a treatment velocity of 0.5 to 3 - 5 cm/sec and a power density of CO2 laser at (3 - 5) 104 W/cm2. X-ray diffractometry, x-ray mapping and Auger electron spectroscopy techniques indicated a TiN phase on the surface with oxygen content 12 - 25 at%. The thickness of the TiN film was 0.3 - 0.4 micrometers after treatment of the 5 micrometers Ti coating and about 900 angstroms for the 0.3 micrometers coating. Some characteristics of TiN films were examined and features of the nitriding process are discussed.

Method for characterization of a spherically bent crystal for K.alpha. X-ray imaging of laser plasmas using a focusing monochromator geometry

DOEpatents

Kugland, Nathan; Doeppner, Tilo; Glenzer, Siegfried; Constantin, Carmen; Niemann, Chris; Neumayer, Paul

2015-04-07

A method is provided for characterizing spectrometric properties (e.g., peak reflectivity, reflection curve width, and Bragg angle offset) of the K.alpha. emission line reflected narrowly off angle of the direct reflection of a bent crystal and in particular of a spherically bent quartz 200 crystal by analyzing the off-angle x-ray emission from a stronger emission line reflected at angles far from normal incidence. The bent quartz crystal can therefore accurately image argon K.alpha. x-rays at near-normal incidence (Bragg angle of approximately 81 degrees). The method is useful for in-situ calibration of instruments employing the crystal as a grating by first operating the crystal as a high throughput focusing monochromator on the Rowland circle at angles far from normal incidence (Bragg angle approximately 68 degrees) to make a reflection curve with the He-like x-rays such as the He-.alpha. emission line observed from a laser-excited plasma.

Crystallization and preliminary X-ray studies of a non-haemorrhagic fibrin(ogen)olytic metalloproteinase from the venom of Agkistrodon acutus

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

Hou, Jing; Li, Ming; Chen, Jiashu

Crystals of a non-haemorrhagic fibrin(ogen)olytic metalloproteinase from the venom of A. acutus have been obtained and characterized by X-ray diffraction. A non-haemorrhagic fibrin(ogen)olytic metalloproteinase from the venom of Agkistrodon acutus has been crystallized by the hanging-drop method. The crystals belong to space group P3{sub 1}21, with unit-cell parameters a = b = 80.57, c = 66.77 Å and one molecule in the asymmetric unit. X-ray diffraction data were collected to 1.86 Å resolution.

Crystallization and X-ray diffraction analysis of a catalytic domain of hyperthermophilic chitinase from Pyrococcus furiosus

PubMed Central

Mine, Shouhei; Nakamura, Tsutomu; Hirata, Kunio; Ishikawa, Kazuhiko; Hagihara, Yoshihisa; Uegaki, Koichi

2006-01-01

The crystallization and preliminary X-ray diffraction analysis of a catalytic domain of chitinase (PF1233 gene) from the hyperthermophilic archaeon Pyrococcus furiosus is reported. The recombinant protein, prepared using an Escherichia coli expression system, was crystallized by the hanging-drop vapour-diffusion method. An X-ray diffraction data set was collected at the undulator beamline BL44XU at SPring-8 to a resolution of 1.50 Å. The crystals belong to space group P212121, with unit-cell parameters a = 90.0, b = 92.8, c = 107.2 Å. PMID:16880559

Ethanol fixed brain imaging by phase-contrast X-ray technique

NASA Astrophysics Data System (ADS)

Takeda, Tohoru; Thet-Thet-Lwin; Kunii, Takuya; Sirai, Ryota; Ohizumi, Takahito; Maruyama, Hiroko; Hyodo, Kazuyuki; Yoneyama, Akio; Ueda, Kazuhiro

2013-03-01

The two-crystal phase-contrast X-ray imaging technique using an X-ray crystal interferometer can depict the fine structures of rat's brain such as cerebral cortex, white matter, and basal ganglia. Image quality and contrast by ethanol fixed brain showed significantly better than those by usually used formalin fixation at 35 keV X-ray energy. Image contrast of cortex by ethanol fixation was more than 3-times higher than that by formalin fixation. Thus, the technique of ethanol fixation might be better suited to image cerebral structural detail at 35 keV X-ray energy.

Acoustic Injectors for Drop-On-Demand Serial Femtosecond Crystallography.

PubMed

Roessler, Christian G; Agarwal, Rakhi; Allaire, Marc; Alonso-Mori, Roberto; Andi, Babak; Bachega, José F R; Bommer, Martin; Brewster, Aaron S; Browne, Michael C; Chatterjee, Ruchira; Cho, Eunsun; Cohen, Aina E; Cowan, Matthew; Datwani, Sammy; Davidson, Victor L; Defever, Jim; Eaton, Brent; Ellson, Richard; Feng, Yiping; Ghislain, Lucien P; Glownia, James M; Han, Guangye; Hattne, Johan; Hellmich, Julia; Héroux, Annie; Ibrahim, Mohamed; Kern, Jan; Kuczewski, Anthony; Lemke, Henrik T; Liu, Pinghua; Majlof, Lars; McClintock, William M; Myers, Stuart; Nelsen, Silke; Olechno, Joe; Orville, Allen M; Sauter, Nicholas K; Soares, Alexei S; Soltis, S Michael; Song, Heng; Stearns, Richard G; Tran, Rosalie; Tsai, Yingssu; Uervirojnangkoorn, Monarin; Wilmot, Carrie M; Yachandra, Vittal; Yano, Junko; Yukl, Erik T; Zhu, Diling; Zouni, Athina

2016-04-05

X-ray free-electron lasers (XFELs) provide very intense X-ray pulses suitable for macromolecular crystallography. Each X-ray pulse typically lasts for tens of femtoseconds and the interval between pulses is many orders of magnitude longer. Here we describe two novel acoustic injection systems that use focused sound waves to eject picoliter to nanoliter crystal-containing droplets out of microplates and into the X-ray pulse from which diffraction data are collected. The on-demand droplet delivery is synchronized to the XFEL pulse scheme, resulting in X-ray pulses intersecting up to 88% of the droplets. We tested several types of samples in a range of crystallization conditions, wherein the overall crystal hit ratio (e.g., fraction of images with observable diffraction patterns) is a function of the microcrystal slurry concentration. We report crystal structures from lysozyme, thermolysin, and stachydrine demethylase (Stc2). Additional samples were screened to demonstrate that these methods can be applied to rare samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Visualization of membrane protein crystals in lipid cubic phase using X-ray imaging

PubMed Central

Warren, Anna J.; Armour, Wes; Axford, Danny; Basham, Mark; Connolley, Thomas; Hall, David R.; Horrell, Sam; McAuley, Katherine E.; Mykhaylyk, Vitaliy; Wagner, Armin; Evans, Gwyndaf

2013-01-01

The focus in macromolecular crystallography is moving towards even more challenging target proteins that often crystallize on much smaller scales and are frequently mounted in opaque or highly refractive materials. It is therefore essential that X-ray beamline technology develops in parallel to accommodate such difficult samples. In this paper, the use of X-ray microradiography and microtomography is reported as a tool for crystal visualization, location and characterization on the macromolecular crystallography beamlines at the Diamond Light Source. The technique is particularly useful for microcrystals and for crystals mounted in opaque materials such as lipid cubic phase. X-ray diffraction raster scanning can be used in combination with radiography to allow informed decision-making at the beamline prior to diffraction data collection. It is demonstrated that the X-ray dose required for a full tomography measurement is similar to that for a diffraction grid-scan, but for sample location and shape estimation alone just a few radiographic projections may be required. PMID:23793151

Visualization of membrane protein crystals in lipid cubic phase using X-ray imaging.

PubMed

Warren, Anna J; Armour, Wes; Axford, Danny; Basham, Mark; Connolley, Thomas; Hall, David R; Horrell, Sam; McAuley, Katherine E; Mykhaylyk, Vitaliy; Wagner, Armin; Evans, Gwyndaf

2013-07-01

The focus in macromolecular crystallography is moving towards even more challenging target proteins that often crystallize on much smaller scales and are frequently mounted in opaque or highly refractive materials. It is therefore essential that X-ray beamline technology develops in parallel to accommodate such difficult samples. In this paper, the use of X-ray microradiography and microtomography is reported as a tool for crystal visualization, location and characterization on the macromolecular crystallography beamlines at the Diamond Light Source. The technique is particularly useful for microcrystals and for crystals mounted in opaque materials such as lipid cubic phase. X-ray diffraction raster scanning can be used in combination with radiography to allow informed decision-making at the beamline prior to diffraction data collection. It is demonstrated that the X-ray dose required for a full tomography measurement is similar to that for a diffraction grid-scan, but for sample location and shape estimation alone just a few radiographic projections may be required.

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

Fukao, Shinji; Nakanishi, Yoshikazu; Mizoguchi, Tadahiro

X-rays are radiated due to the bremsstrahlung caused by the collision of electrons with a metal target placed opposite the negative electric surface of a crystal by changing the temperature of a LiNbO{sub 3} single crystal uniaxially polarized in the c-axis direction. It is suggested that both electric field intensity and electron density determine the intensity of X-ray radiation. Electrons are supplied by the ionization of residual gas in space, field emission from a case inside which a crystal is located, considered to be due to the high electric-field intensity formed by the surface charges on the crystal, and anmore » external electron source, such as a thermionic source. In a high vacuum, it was found that the electrons supplied by electric-field emission mainly contribute to the radiation of X-rays. It was found that the integrated intensity of X-rays can be maximized by supplying electrons both external and by electric-field emission. Furthermore, the integrated intensity of the X-rays is stable for many repeated temperature changes.« less

X-ray transparent microfluidic chip for mesophase-based crystallization of membrane proteins and on-chip structure determination

DOE PAGES

Khvostichenko, Daria S.; Schieferstein, Jeremy M.; Pawate, Ashtamurthy S.; ...

2014-08-21

Crystallization from lipidic mesophase matrices is a promising route to diffraction-quality crystals and structures of membrane proteins. The microfluidic approach reported here eliminates two bottlenecks of the standard mesophase-based crystallization protocols: (i) manual preparation of viscous mesophases and (ii) manual harvesting of often small and fragile protein crystals. In the approach reported here, protein-loaded mesophases are formulated in an X-ray transparent microfluidic chip using only 60 nL of the protein solution per crystallization trial. The X-ray transparency of the chip enables diffraction data collection from multiple crystals residing in microfluidic wells, eliminating the normally required manual harvesting and mounting ofmore » individual crystals. In addition, we validated our approach by on-chip crystallization of photosynthetic reaction center, a membrane protein from Rhodobacter sphaeroides, followed by solving its structure to a resolution of 2.5 Å using X-ray diffraction data collected on-chip under ambient conditions. A moderate conformational change in hydrophilic chains of the protein was observed when comparing the on-chip, room temperature structure with known structures for which data were acquired under cryogenic conditions.« less

X-ray Transparent Microfluidic Chip for Mesophase-Based Crystallization of Membrane Proteins and On-Chip Structure Determination

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

Khvostichenko, Daria S.; Schieferstein, Jeremy M.; Pawate, Ashtamurthy S.

2014-10-01

Crystallization from lipidic mesophase matrices is a promising route to diffraction-quality crystals and structures of membrane proteins. The microfluidic approach reported here eliminates two bottlenecks of the standard mesophase-based crystallization protocols: (i) manual preparation of viscous mesophases and (ii) manual harvesting of often small and fragile protein crystals. In the approach reported here, protein-loaded mesophases are formulated in an X-ray transparent microfluidic chip using only 60 nL of the protein solution per crystallization trial. The X-ray transparency of the chip enables diffraction data collection from multiple crystals residing in microfluidic wells, eliminating the normally required manual harvesting and mounting ofmore » individual crystals. We validated our approach by on-chip crystallization of photosynthetic reaction center, a membrane protein from Rhodobacter sphaeroides, followed by solving its structure to a resolution of 2.5 Å using X-ray diffraction data collected on-chip under ambient conditions. A moderate conformational change in hydrophilic chains of the protein was observed when comparing the on-chip, room temperature structure with known structures for which data were acquired under cryogenic conditions.« less

Effects of thermal expansion of the crystal lattice on x-ray crystal spectrometers used for fusion research

NASA Astrophysics Data System (ADS)

Delgado-Aparicio, L.; Bitter, M.; Podpaly, Y.; Rice, J.; Burke, W.; Sanchez del Rio, M.; Beiersdorfer, P.; Bell, R.; Feder, R.; Gao, C.; Hill, K.; Johnson, D.; Lee, S. G.; Marmar, E.; Pablant, N.; Reinke, M. L.; Scott, S.; Wilson, R.

2013-12-01

X-ray imaging crystal spectrometers with high spectral and spatial resolution are currently being used on magnetically confined fusion devices to infer the time history profiles of ion and electron temperatures as well as plasma flow velocities. The absolute measurement of flow velocities is important for optimizing various discharge scenarios and evaluating the radial electric field in tokamak and stellarator plasmas. Recent studies indicate that the crystal temperature must be kept constant to within a fraction of a degree to avoid changes of the interplanar 2d-spacing by thermal expansion that cause changes in the Bragg angle, which could be misinterpreted as Doppler shifts. For the instrumental parameters of the x-ray crystal spectrometer on Alcator C-Mod, where those thermal effects were investigated, a change of the crystal temperature by 1 °C causes a change of the lattice spacing of the order of Δd = 1 × 10-5 Å introducing a fictitious velocity drift of the order of ˜3 km s-1. This effect must be considered for x-ray imaging crystals spectrometers installed on LHD, KSTAR, EAST, J-TEXT, NSTX and, in the future, W7-X and ITER.

The Ferrara hard X-ray facility for testing/calibrating hard X-ray focusing telescopes

NASA Astrophysics Data System (ADS)

Loffredo, Gianluca; Frontera, Filippo; Pellicciotta, Damiano; Pisa, Alessandro; Carassiti, Vito; Chiozzi, Stefano; Evangelisti, Federico; Landi, Luca; Melchiorri, Michele; Squerzanti, Stefano

2005-12-01

We will report on the current configuration of the X-ray facility of the University of Ferrara recently used to perform reflectivity tests of mosaic crystals and to calibrate the experiment JEM X aboard Integral. The facility is now located in the technological campus of the University of Ferrara in a new building (named LARIX laboratory= LARge Italian X-ray facility) that includes a tunnel 100 m long with, on the sides, two large experimental rooms. The facility is being improved for determining the optical axis of mosaic crystals in Laue configuration, for calibrating Laue lenses and hard X-ray mirror prototypes.

Preliminary morphological and X-ray diffraction studies of the crystals of the DNA cetyltrimethylammonium salt.

PubMed

Osica, V D; Pyatigorskaya, T L; Polyvtsev, O F; Dembo, A T; Kliya, M O; Vasilchenko, V N; Verkin, B I; Sukharevskya, B Y

1977-04-01

Double-stranded DNA molecules (molecular weight 2.5 X 10(5) - 5 X 10(5) daltons) have been crystallized from water-salt solutions as cetyltrimethylammonium salts (CTA-DNA). Variation of crystallization conditions results in a production of different types of CTA-DNA crystals: spherulits, dendrites, needle-shaped and faceted rhombic crystals, the latter beeing up to 0.3 mm on a side. X-ray diffraction data indicate that DNA molecules in the crystals form a hexagonal lattice which parameters vary slightly with the morphological type of the crystal. Comparison of the melting curves of the DNA preparation before and after crystallization suggests that DNA molecules are partially fractionated in the course of crystallization. Crystals of the CTA-DNA-proflavine complex have also been obtained.

Preliminary morphological and X-ray diffraction studies of the crystals of the DNA cetyltrimethylammonium salt.

PubMed Central

Osica, V D; Pyatigorskaya, T L; Polyvtsev, O F; Dembo, A T; Kliya, M O; Vasilchenko, V N; Verkin, B I; Sukharevskya, B Y

1977-01-01

Double-stranded DNA molecules (molecular weight 2.5 X 10(5) - 5 X 10(5) daltons) have been crystallized from water-salt solutions as cetyltrimethylammonium salts (CTA-DNA). Variation of crystallization conditions results in a production of different types of CTA-DNA crystals: spherulits, dendrites, needle-shaped and faceted rhombic crystals, the latter beeing up to 0.3 mm on a side. X-ray diffraction data indicate that DNA molecules in the crystals form a hexagonal lattice which parameters vary slightly with the morphological type of the crystal. Comparison of the melting curves of the DNA preparation before and after crystallization suggests that DNA molecules are partially fractionated in the course of crystallization. Crystals of the CTA-DNA-proflavine complex have also been obtained. Images PMID:866188

X-ray evaluation of crystals for stellar spectrometers

NASA Technical Reports Server (NTRS)

Alexandropolos, N. G. (Editor)

1974-01-01

The report consists of three parts. The first part is an analysis of the principles involved in X-ray crystal evaluation and how they are applied to a number of crystals. The principles of crystal evaluation analysis as they apply to the special problems of X-ray astronomy are presented. A number of crystals were evaluated, and the energy dependence of the diffraction properties of (002) PET, (111) Ge, (101) ADP, (001) KAP, and (001) RAP are reported. The second part is a compilation of the diffraction properties of a number of crystals as reported by other authors. In the third part some technical details of a triple crystal spectrometer built by the author at Polytechnic Institute of Brooklyn are given. This spectrometer seems to be a most appropriate instrument for evaluation of crystal properties. (Modified author abstract)

Photonic crystals at visible, x-ray, and terahertz frequencies

NASA Astrophysics Data System (ADS)

Prasad, Tushar

Photonic crystals are artificial structures with a periodically varying refractive index. This property allows photonic crystals to control the propagation of photons, making them desirable components for novel photonic devices. Photonic crystals are also termed as "semiconductors of light", since they control the flow of electromagnetic radiation similar to the way electrons are excited in a semiconductor crystal. The scale of periodicity in the refractive index determines the frequency (or wavelength) of the electromagnetic waves that can be manipulated. This thesis presents a detailed analysis of photonic crystals at visible, x-ray, and terahertz frequencies. Self-assembly and spin-coating methods are used to fabricate colloidal photonic crystals at visible frequencies. Their dispersion characteristics are examined through theoretical as well as experimental studies. Based on their peculiar dispersion property called the superprism effect, a sensor that can detect small quantities of chemical substances is designed. A photonic crystal that can manipulate x-rays is fabricated by using crystals of a non-toxic plant virus as templates. Calculations show that these metallized three-dimensional crystals can find utility in x-ray optical systems. Terahertz photonic crystal slabs are fabricated by standard lithographic and etching techniques. In-plane superprism effect and out-of-plane guided resonances are studied by terahertz time-domain spectroscopy, and verified by numerical simulations.

A multi-cone x-ray imaging Bragg crystal spectrometer

DOE PAGES

Bitter, M.; Hill, K. W.; Gao, Lan; ...

2016-08-26

This article describes a new x-ray imaging Bragg crystal spectrometer, which—in combination with a streak camera or a gated strip detector—can be used for time-resolved measurements of x-ray line spectra at the National Ignition Facility and other high power laser facilities. The main advantage of this instrument is that it produces perfect images of a point source for each wavelength in a selectable spectral range and that the detector plane can be perpendicular to the crystal surface or inclined by an arbitrary angle with respect to the crystal surface. Furthermore, these unique imaging properties are obtained by bending the x-raymore » diffracting crystal into a certain shape, which is generated by arranging multiple cones with different aperture angles on a common nodal line.« less

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

Pratapa, S.; Susanti, L.; Insany, Y. A. S.

Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgO{center_dot}Al{sub 2}O{sub 3}(spinel), Y{sub 2}O{sub 3}(yttria) and Fe{sub 3}O{sub 4}(ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100 deg. C, followed by heating at 450 deg. C, 750 deg. C, 600 deg. C and 200 deg.more » C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited 'longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as 'fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.« less

Mineralogical variation in the size fractions of a Ranong kaolin, southern Thailand

NASA Astrophysics Data System (ADS)

Pisutha-Arnond, Visut; Phuvichit, Suraphol; Leepowpanth, Quanchai

A representative crude Ranong kaolin from the Thungkla-Ranong mine was separated into > 2 mm (granule), 2-1 mm (very coarse sand), 1-0.5 mm (coarse sand), 0.5-0.25 mm (medium sand), 0.25-0.125 mm (fine sand), 0.125-0.062 mm (very fine sand) and 62-28, 28-14, 17-7, 7-4, 4-2, 2-1 and < 1 μ m size fractions. Those size fractions were analyzed by X-ray powder diffractometry (XRD), differential thermal analysis (DTA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) with attached energy dispersive X-ray spectrometer (EDX). Kaolin group minerals were differentiated by using XRD in combination with various chemical and heat treatments together with TEM, SEM and DTA. The Ranong kaolin consists predominantly of tubular halloysite, poorly crystallized kaolinite and quartz with minor amounts of mica and K-feldspars. Other trace constituents include gibbsite, tourmaline, zircon and colored impurities (i.e. extractable iron hydroxide coating on clay mineral surface). The kaolin minerals are found in all size fractions by which their contents and halloysite/kaolinite ratios increase as the particle sizes become finer. Quartz and mica are also detected in almost all size fractions. They are, however, more abundant with coarsening particle size. Gibbsite, K-feldspar and tourmaline are mainly concentrated in the fine sand to silt size fractions. Crystallinity of kaolin minerals as measured by XRD varied moderately with size. Relatively pure kaolin minerals, predominantly halloysite and kaolinite, can be obtained in the particle size below 1 or 2 μm.

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

NASA Technical Reports Server (NTRS)

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

2010-01-01

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

Characterization of two polymorphs of salmeterol xinafoate crystallized from supercritical fluids.

PubMed

Tong, H H; Shekunov, B Y; York, P; Chow, A H

2001-06-01

To characterize two polymorphs of salmeterol xinafoate (SX-I and SX-II) produced by supercritical fluid crystallization. SX-I and SX-II were crystallized as fine powders using Solution Enhanced Dispersion by Supercritical Fluids (SEDS). The two polymorphs and a reference micronized SX sample (MSX) were characterized using powder X-ray diffractometry (PXRD), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), aqueous solubility (and dissolution) determination at 5-40 degrees C, BET adsorption analysis, and inverse gas chromatography (IGC). Compared with SX-I, SX-II exhibited a lower enthalpy of fusion, a higher equilibrium solubility, a higher intrinsic dissolution rate, a lower enthalpy of solution (based on van't Hoff solubility plots), and a different FTIR spectrum (reflecting differences in intermolecular hydrogen bonding). Solubility ratio plot yielded a transition temperature (-99 degrees C) below the melting points of both polymorphs. MSX showed essentially the same crystal form as SX-I (confirmed by PXRD and FTIR), but a distinctly different thermal behaviour. Mild trituration of SX-I afforded a similar DSC profile to MSX while prolonged grinding of SX-I gave rise to an endotherm at -109 degrees C, corresponding to solid-solid transition of SX-I to SX-II. Surface analysis of MSX, SX-I, and SX-II by IGC revealed significant differences in surface free energy in terms of both dispersive (nonpolar) interactions and specific (polar) acid-base properties. The SEDS-processed SX-I and SX-II display high polymorphic purity and distinctly different physical and surface properties. The polymorphs are related enantiotropically with SX-I being the thermodynamically stable form at room temperature.

Synthesis and Characterization of Cobalt Substituted Zinc Ferrite Nanoparticles by Microwave Combustion Method.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith

2015-09-01

Pure and cobalt doped zinc ferrites were prepared by microwave combustion method using L-arginine as a fuel. The prepared samples were characterized by various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis, Fourier transformed infrared (FT-IR) spectroscopy, photoluminescence spectroscopy and UV-Visible diffuse reflectance spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis confirmed the formation of zinc ferrites normal spinel-type structure with an average crystallite sizes in the range, 25.69 nm to 35.68 nm. The lattice parameters decreased as cobalt fraction was increased. The HR-SEM images showed nanoparticles are agglomerated. The estimated band gap energy value was found to decrease with an increase in cobalt content (1.87 to 1.62 eV). Broad visible emissions are observed in the photoluminescence spectra. A gradual increase in the coercivity and saturation magnetization (M(s)) were noted at relatively higher cobalt doping fractions.

From nicotinate-containing layered double hydroxides (LDHs) to NAD coenzyme-LDH nanocomposites - Syntheses and structural characterization by various spectroscopic methods

NASA Astrophysics Data System (ADS)

Muráth, Szabolcs; Dudás, Csilla; Kukovecz, Ákos; Kónya, Zoltán; Sipos, Pál; Pálinkó, István

2017-07-01

The syntheses of nicotinate anion- and NAD coenzyme-layered double hydroxide (LDH) composites were performed with the aim of having the organic component among the layers. In-house prepared CaAl-LDHs were the host materials. Intercalation was attempted by direct ion exchange or by the dehydration-rehydration method applying aqueous solvent mixtures (containing ethanol, propanol, acetone, N,N-dimethylformamide). For structural characterization, beside X-ray diffractometry, X-ray photoelectron and IR spectroscopies, transmission and scanning electron microscopies as well as energy-dispersive X-ray analysis were used. Molecular modelling served for the visualization of the arrangements of the intercalated ions among the layers of the LDH samples. Although not all the intercalation methods and solvent mixtures led to intercalated composite materials, successful ones could be identified. The combination of spectroscopic methods helped in proposing sensible spatial arrangements for the intercalated anions. The NAD-CaAl-LDH composite proved to be an active catalyst in the oxidation of hydroquinone to 1,4-bezoquinoe in the presence of H2O2.

Ultrasonically-enhanced preparation, characterization of CaFe-layered double hydroxides with various interlayer halide, azide and oxo anions (CO32-, NO3-, ClO4-).

PubMed

Szabados, Márton; Varga, Gábor; Kónya, Zoltán; Kukovecz, Ákos; Carlson, Stefan; Sipos, Pál; Pálinkó, István

2018-01-01

An ultrasonically-enhanced mechanochemical method was developed to synthesize CaFe-layered double hydroxides (LDHs) with various interlayer anions (CO 3 2- , NO 3 - , ClO 4 - , N 3 - , F - , Cl - , Br - and I - ). The duration of pre-milling and ultrasonic irradiation and the variation of synthesis temperature in the wet chemical step were investigated to obtain the optimal parameters of preparation. The main method to characterize the products was X-ray diffractometry, but infrared and synchrotron-based X-ray absorption spectroscopies as well as thermogravimetric measurements were also used to learn about fine structural details. The synthesis method afforded successful intercalation of the anions, among others the azide anion, a rarely used counter ion providing a system, which enables safe handling the otherwise highly reactive anion. The X-ray absorption spectroscopic measurements revealed that the quality of the interlayered anions could modulate the spatial arrangement of the calcium ions around the iron(III) ions, but only in the second coordination sphere. Copyright © 2017 Elsevier B.V. All rights reserved.

Preliminary small-angle X-ray scattering and X-ray diffraction studies of the BTB domain of lola protein from Drosophila melanogaster

NASA Astrophysics Data System (ADS)

Boyko, K. M.; Nikolaeva, A. Yu.; Kachalova, G. S.; Bonchuk, A. N.; Dorovatovskii, P. V.; Popov, V. O.

2017-11-01

The Drosophila genome has several dozens of transcription factors (TTK group) containing BTB domains assembled into octamers. The LOLA protein belongs to this family. The purification, crystallization, and preliminary X-ray diffraction and small-angle X-ray scattering (SAXS) studies of the BTB domain of this protein are reported. The crystallization conditions were found by the vapor-diffusion technique. A very low diffraction resolution (8.7 Å resolution) of the crystals was insufficient for the determination of the threedimensional structure of the BTB domain. The SAXS study demonstrated that the BTB domain of the LOLA protein exists as an octamer in solution.

One-shot spectrometer for several elements using an integrated conical crystal analyzer

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

Morishita, Kohei; Nakajima, Kazuo; Hayashi, Kouichi

Time-resolved x-ray spectrometry using an ultrastrong x-ray source such as an x-ray free electron laser is one of the new trends in the field of x-ray physics. To achieve such time-resolved measurement, the development of an one-shot spectrometer with a wide wavelength range, high efficiency, and good energy resolution is an essential prerequisite. Here we developed an integrated conical Ge crystal analyzer consisting of several conical rings, which were connected using spline surfaces to form a single body using our previously developed hot deformation technique, which can form a Si or Ge wafer into an arbitrary and accurate shape. Wemore » simultaneously focused several characteristic lines from an alloy sample onto different positions on a small x-ray charge-coupled device with very high image brightness (gain relative to planar analyzer: 100) and a good spatial resolution of 9-13 eV. The small radius of curvature of the crystal (28-50 mm) enabled us to realize a very short sample-detector distance of 214.4 mm. The present result shows the possibility of realizing a new focusing x-ray crystal spectrograph that can control the focal position as desired.« less

Diffraction and Imaging Study of Imperfections of Protein Crystals with Coherent X-rays

NASA Technical Reports Server (NTRS)

Hu, Z. W.; Thomas, B. R.; Chernov, A. A.; Chu, Y. S.; Lai, B.

2004-01-01

High angular-resolution x-ray diffraction and phase contrast x-ray imaging were combined to study defects and perfection of protein crystals. Imperfections including line defects, inclusions and other microdefects were observed in the diffraction images of a uniformly grown lysozyme crystal. The observed line defects carry distinct dislocation features running approximately along the <110> growth front and have been found to originate mostly in a central growth area and occasionally in outer growth regions. Slow dehydration led to the broadening of a fairly symmetric 4 4 0 rocking curve by a factor of approximately 2.6, which was primarily attributed to the dehydration-induced microscopic effects that are clearly shown in diffraction images. X-ray imaging and diffraction characterization of the quality of apoferritin crystals will also be discussed in the presentation.

Laboratory multiple-crystal X-ray topography and reciprocal-space mapping of protein crystals: influence of impurities on crystal perfection

NASA Technical Reports Server (NTRS)

Hu, Z. W.; Thomas, B. R.; Chernov, A. A.

2001-01-01

Double-axis multiple-crystal X-ray topography, rocking-curve measurements and triple-axis reciprocal-space mapping have been combined to characterize protein crystals using a laboratory source. Crystals of lysozyme and lysozyme crystals doped with acetylated lysozyme impurities were examined. It was shown that the incorporation of acetylated lysozyme into crystals of lysozyme induces mosaic domains that are responsible for the broadening and/or splitting of rocking curves and diffraction-space maps along the direction normal to the reciprocal-lattice vector, while the overall elastic lattice strain of the impurity-doped crystals does not appear to be appreciable in high angular resolution reciprocal-space maps. Multiple-crystal monochromatic X-ray topography, which is highly sensitive to lattice distortions, was used to reveal the spatial distribution of mosaic domains in crystals which correlates with the diffraction features in reciprocal space. Discussions of the influence of acetylated lysozyme on crystal perfection are given in terms of our observations.

Laboratory multiple-crystal X-ray topography and reciprocal-space mapping of protein crystals: influence of impurities on crystal perfection.

PubMed

Hu, Z W; Thomas, B R; Chernov, A A

2001-06-01

Double-axis multiple-crystal X-ray topography, rocking-curve measurements and triple-axis reciprocal-space mapping have been combined to characterize protein crystals using a laboratory source. Crystals of lysozyme and lysozyme crystals doped with acetylated lysozyme impurities were examined. It was shown that the incorporation of acetylated lysozyme into crystals of lysozyme induces mosaic domains that are responsible for the broadening and/or splitting of rocking curves and diffraction-space maps along the direction normal to the reciprocal-lattice vector, while the overall elastic lattice strain of the impurity-doped crystals does not appear to be appreciable in high angular resolution reciprocal-space maps. Multiple-crystal monochromatic X-ray topography, which is highly sensitive to lattice distortions, was used to reveal the spatial distribution of mosaic domains in crystals which correlates with the diffraction features in reciprocal space. Discussions of the influence of acetylated lysozyme on crystal perfection are given in terms of our observations.

Surface-treated self-standing curved crystals as high-efficiency elements for X- and γ-ray optics: theory and experiment.

PubMed

Bonnini, Elisa; Buffagni, Elisa; Zappettini, Andrea; Doyle, Stephen; Ferrari, Claudio

2015-06-01

The efficiency of a Laue lens for X- and γ-ray focusing in the energy range 60-600 keV is closely linked to the diffraction efficiency of the single crystals composing the lens. A powerful focusing system is crucial for applications like medical imaging and X-ray astronomy where wide beams must be focused. Mosaic crystals with a high density, such as Cu or Au, and bent crystals with curved diffracting planes (CDPs) are considered for the realization of a focusing system for γ-rays, owing to their high diffraction efficiency in a predetermined angular range. In this work, a comparison of the efficiency of CDP crystals and Cu and Au mosaic crystals was performed on the basis of the theory of X-ray diffraction. Si, GaAs and Ge CDP crystals with optimized thicknesses and moderate radii of curvature of several tens of metres demonstrate comparable or superior performance with respect to the higher atomic number mosaic crystals generally used. In order to increase the efficiency of the lens further, a stack of several CDP crystals is proposed as an optical element. CDP crystals were obtained by a surface-damage method, and a stack of two surface-damaged bent Si crystals was prepared and tested. Rocking curves of the stack were performed with synchrotron radiation at 19 keV to check the lattice alignment: they exhibited only one diffraction peak.

Crystallization and preliminary X-ray analysis of the stress-response PPM phosphatase RsbX from Bacillus subtilis

PubMed Central

Suganuma, Masatoshi; Teh, Aik Hong; Makino, Masatomo; Shimizu, Nobutaka; Kaneko, Tomonori; Hirata, Kunio; Yamamoto, Masaki; Kumasaka, Takashi

2009-01-01

RsbX from Bacillus subtilis is a manganese-dependent PPM phosphatase and negatively regulates the signal transduction of the general stress response by the dephosphorylation of RsbS and RsbR, which are activators of the alternative RNA polymerase σ factor SigB. In order to elucidate the structural–functional relationship of its Ser/Thr protein-phosphorylation mechanism, an X-ray crystallographic diffraction study of RsbX was performed. Recombinant RsbX was expressed in Escherichia coli, purified and crystallized. Crystals were obtained using the sitting-drop vapour-diffusion method and X-ray diffraction data were collected to 1.06 Å resolution with an R merge of 8.1%. The crystals belonged to the triclinic space group P1, with unit-cell parameters a = 33.3, b = 41.7, c = 68.6 Å, α = 98.8, β = 90.0, γ = 108.4°. PMID:19923733

Crystallization and preliminary X-ray analysis of the stress-response PPM phosphatase RsbX from Bacillus subtilis.

PubMed

Suganuma, Masatoshi; Teh, Aik Hong; Makino, Masatomo; Shimizu, Nobutaka; Kaneko, Tomonori; Hirata, Kunio; Yamamoto, Masaki; Kumasaka, Takashi

2009-11-01

RsbX from Bacillus subtilis is a manganese-dependent PPM phosphatase and negatively regulates the signal transduction of the general stress response by the dephosphorylation of RsbS and RsbR, which are activators of the alternative RNA polymerase sigma factor SigB. In order to elucidate the structural-functional relationship of its Ser/Thr protein-phosphorylation mechanism, an X-ray crystallographic diffraction study of RsbX was performed. Recombinant RsbX was expressed in Escherichia coli, purified and crystallized. Crystals were obtained using the sitting-drop vapour-diffusion method and X-ray diffraction data were collected to 1.06 angstrom resolution with an R(merge) of 8.1%. The crystals belonged to the triclinic space group P1, with unit-cell parameters a = 33.3, b = 41.7, c = 68.6 angstrom , alpha = 98.8, beta = 90.0, gamma = 108.4 degrees.

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

Lu, J., E-mail: jlu@pppl.gov; Bitter, M.; Hill, K. W.

A two-dimensional stigmatic x-ray imaging scheme, consisting of two spherically bent crystals, one concave and one convex, was recently proposed [M. Bitter et al., Rev. Sci. Instrum. 83, 10E527 (2012)]. The Bragg angles and the radii of curvature of the two crystals of this imaging scheme are matched to eliminate the astigmatism and to satisfy the Bragg condition across both crystal surfaces for a given x-ray energy. In this paper, we consider more general configurations of this imaging scheme, which allow us to vary the magnification for a given pair of crystals and x-ray energy. The stigmatic imaging scheme hasmore » been validated for the first time by imaging x-rays generated by a micro-focus x-ray source with source size of 8.4 μm validated by knife-edge measurements. Results are presented from imaging the tungsten Lα1 emission at 8.3976 keV, using a convex Si-422 crystal and a concave Si-533 crystal with 2d-spacings of 2.21707 Å and 1.65635 Å and radii of curvature of 500 ± 1 mm and 823 ± 1 mm, respectively, showing a spatial resolution of 54.9 μm. This imaging scheme is expected to be of interest for the two-dimensional imaging of laser produced plasmas.« less

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

Lu, J.; Bitter, M.; Hill, K. W.

A two-dimensional stigmatic x-ray imaging scheme, consisting of two spherically bent crystals, one concave and one convex, was recently proposed [M. Bitter et al., Rev. Sci. Instrum. 83, 10E527 (2012)]. We report that the Bragg angles and the radii of curvature of the two crystals of this imaging scheme are matched to eliminate the astigmatism and to satisfy the Bragg condition across both crystal surfaces for a given x-ray energy. In this paper, we consider more general configurations of this imaging scheme, which allow us to vary the magnification for a given pair of crystals and x-ray energy. The stigmaticmore » imaging scheme has been validated for the first time by imaging x-rays generated by a micro-focus x-ray source with source size of 8.4 μm validated by knife-edge measurements. Results are presented from imaging the tungsten Lα1 emission at 8.3976 keV, using a convex Si-422 crystal and a concave Si-533 crystal with 2d-spacings of 2.21707 Å and 1.65635 Å and radii of curvature of 500 ± 1 mm and 823 ± 1 mm, respectively, showing a spatial resolution of 54.9 μm. Finally, this imaging scheme is expected to be of interest for the two-dimensional imaging of laser produced plasmas.« less

High spatial resolution X-ray and gamma ray imaging system using diffraction crystals

DOEpatents

Smither, Robert K [Hinsdale, IL

2011-05-17

A method and a device for high spatial resolution imaging of a plurality of sources of x-ray and gamma-ray radiation are provided. The device comprises a plurality of arrays, with each array comprising a plurality of elements comprising a first collimator, a diffracting crystal, a second collimator, and a detector.

Crystallization of belite–melilite clinker minerals in the presence of liquid phase

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

Kurokawa, Daisuke, E-mail: daisuke_kurokawa@taiheiyo-cement.co.jp; Department of Materials Science and Engineering, Nagoya Institute of Technology, Nagoya 466-8555; Yoshida, Hideto

2014-06-01

Crystallization of belite–melilite clinker minerals was studied from the view point of a high temperature equilibrium. Ca{sub 2}SiO{sub 4}–Ca{sub 2}Al{sub 2}SiO{sub 7} and Ca{sub 2}SiO{sub 4}–Ca{sub 2}AlFeSiO{sub 7} clinkers were synthesized at 1330 °C–1650 °C. The constituent phases were determined by X-ray powder diffractometry and optical microscopy. Chemical compositions of the individual clinker minerals were determined using an electron probe microanalyzer. We established the two types of P{sub 2}O{sub 5}-bearing pseudobinary phase diagrams in the systems Ca{sub 2}SiO{sub 4}–Ca{sub 2}Al{sub 2}SiO{sub 7} at 1505 °C–1650 °C and Ca{sub 2}SiO{sub 4}–Ca{sub 2}(Al,Fe){sub 2}SiO{sub 7} at 1330 °C–1550 °C. In the lattermore » system, the liquid phase appeared at 1390 °C, which is approximately 150 °C lower than the temperature of liquid formation in the former system. The melilite phenocrysts larger than 50 μm were observed not only in the slowly cooled Ca{sub 2}SiO{sub 4}–Ca{sub 2}(Al,Fe){sub 2}SiO{sub 7} clinker but also in commercial belite–melilite clinkers. These crystals would be nucleated and grown from a liquid phase which was formed at relatively low temperatures.« less

First X-ray crystal structure and internal reference diffusion-ordered NMR spectroscopy study of the prototypical Posner reagent, MeCu(SPh)Li(THF)3.

PubMed

Bertz, Steven H; Hardin, Richard A; Heavey, Thomas J; Jones, Daniel S; Monroe, T Blake; Murphy, Michael D; Ogle, Craig A; Whaley, Tara N

2013-07-29

Grow slow: The usual direct treatment of MeLi and CuSPh did not yield X-ray quality crystals of MeCu(SPh)Li. An indirect method starting from Me2CuLi⋅LiSPh and chalcone afforded the desired crystals by the slow reaction of the intermediate π-complex (see scheme). This strategy produced the first X-ray crystal structure of a Posner cuprate. A complementary NMR study showed that the contact ion pair was also the main species in solution. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Diffraction imaging for in situ characterization of double-crystal X-ray monochromators

DOE PAGES

Stoupin, Stanislav; Liu, Zunping; Heald, Steve M.; ...

2015-10-30

In this paper, imaging of the Bragg-reflected X-ray beam is proposed and validated as an in situ method for characterization of the performance of double-crystal monochromators under the heat load of intense synchrotron radiation. A sequence of images is collected at different angular positions on the reflectivity curve of the second crystal and analyzed. The method provides rapid evaluation of the wavefront of the exit beam, which relates to local misorientation of the crystal planes along the beam footprint on the thermally distorted first crystal. The measured misorientation can be directly compared with the results of finite element analysis. Finally,more » the imaging method offers an additional insight into the local intrinsic crystal quality over the footprint of the incident X-ray beam.« less

Crystallization and preliminary X-ray analysis of gamma-glutamyltranspeptidase from Escherichia coli K-12.

PubMed

Kumagai, H; Nohara, S; Suzuki, H; Hashimoto, W; Yamamoto, K; Sakai, H; Sakabe, K; Fukuyama, K; Sakabe, N

1993-12-20

gamma-Glutamyltranspeptidase (EC 2.3.2.2) from Escherichia coli K-12 has been purified and crystallized by means of vapor diffusion in hanging drops. Two kinds of crystals on cell dimensions were found for X-ray diffraction analysis, one from ammonium sulfate and the other from polyethylene glycol 6000 as precipitants. The crystals of the orthorhombic form grown in the presence of 15% polyethylene glycol and 20 mM sodium acetate buffer were chosen for further analysis. The crystals belonged to space group P2(1)2(1)2(1), with cell dimensions of a = 128.1, b = 129.9 and c = 79.2 A, and two molecules constitute an asymmetric unit. These crystals diffracted to 2.0 A resolution and were suitable for X-ray crystallographic studies.

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

PubMed

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

2015-02-25

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

Simulating Picosecond X-ray Diffraction from shocked crystals by Post-processing Molecular Dynamics Calculations

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

Kimminau, G; Nagler, B; Higginbotham, A

2008-06-19

Calculations of the x-ray diffraction patterns from shocked crystals derived from the results of Non-Equilibrium-Molecular-Dynamics (NEMD) simulations are presented. The atomic coordinates predicted by the NEMD simulations combined with atomic form factors are used to generate a discrete distribution of electron density. A Fast-Fourier-Transform (FFT) of this distribution provides an image of the crystal in reciprocal space, which can be further processed to produce quantitative simulated data for direct comparison with experiments that employ picosecond x-ray diffraction from laser-irradiated crystalline targets.

Simulations of Beam Optics and Bremsstrahlung for High Intensity and Brightness Channeling Radiation

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

Hyun, J.; Piot, P.; Sen, T.

2018-04-12

This paper presents X-ray spectra of channeling radiation expected at the FAST (Fermi Accelerator Science and Technology) facility in Fermilab. Our purpose is to produce high brightness quasi-monochromatic X-rays in an energy range from 40 keV to 110 keV. We will use a diamond crystal and low emittance electrons with an energy of around 43 MeV. The quality of emitted X-rays depends on parameters of the electron beam at the crystal. We present simulations of the beam optics for high brightness and high yield operations for a range of bunch charges. We estimate the X-ray spectra including bremsstrahlung background. Wemore » discuss how the electron beam distributions after the diamond crystal are affected by channeling. We discuss an X-ray detector system to avoid pile-up effects during high charge operations.« less

Simulations of Beam Optics and Bremsstrahlung for High Intensity and Brightness Channeling Radiation

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

Hyun, J.; Piot, P.; Sen, T.

This paper presents X-ray spectra of channeling radiation expected at the FAST (Fermi Accelerator Science and Technology) facility in Fermilab. Our purpose is to produce high brightness quasi-monochromatic X-rays in an energy range from 40 keV to 110 keV. We will use a diamond crystal and low emittance electrons with an energy of around 43 MeV. The quality of emitted X-rays depends on parameters of the electron beam at the crystal. We present simulations of the beam optics for high brightness and high yield operations for a range of bunch charges. We estimate the X-ray spectra including bremsstrahlung background. Wemore » discuss how the electron beam distributions after the diamond crystal are affected by channeling. Here, we discuss an X-ray detector system to avoid pile-up effects during high charge operations.« less

Simulations of Beam Optics and Bremsstrahlung for High Intensity and Brightness Channeling Radiation

DOE PAGES

Hyun, J.; Piot, P.; Sen, T.

2018-06-14

This paper presents X-ray spectra of channeling radiation expected at the FAST (Fermi Accelerator Science and Technology) facility in Fermilab. Our purpose is to produce high brightness quasi-monochromatic X-rays in an energy range from 40 keV to 110 keV. We will use a diamond crystal and low emittance electrons with an energy of around 43 MeV. The quality of emitted X-rays depends on parameters of the electron beam at the crystal. We present simulations of the beam optics for high brightness and high yield operations for a range of bunch charges. We estimate the X-ray spectra including bremsstrahlung background. Wemore » discuss how the electron beam distributions after the diamond crystal are affected by channeling. Here, we discuss an X-ray detector system to avoid pile-up effects during high charge operations.« less

Theoretical calculation of coherent Laue-case conversion between x-rays and ALPs for an x-ray light-shining-through-a-wall experiment

NASA Astrophysics Data System (ADS)

Yamaji, T.; Yamazaki, T.; Tamasaku, K.; Namba, T.

2017-12-01

Single crystals have high atomic electric fields as much as 1 011 V /m , which correspond to magnetic fields of ˜103 T . These fields can be utilized to convert x-rays into axionlike particles (ALPs) coherently similar to x-ray diffraction. In this paper, we perform the first theoretical calculation of the Laue-case conversion in crystals based on the Darwin dynamical theory of x-ray diffraction. The calculation shows that the Laue-case conversion has longer interaction length than the Bragg case, and that ALPs in the keV range can be resonantly converted by tuning an incident angle of x-rays. ALPs with mass up to O (10 keV ) can be searched by light-shining-through-a-wall (LSW) experiments at synchrotron x-ray facilities.

Correct interpretation of diffraction properties of quartz crystals for X-ray optics applications

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

Huang, Xian-Rong; Gog, Thomas; Kim, Jungho

Quartz has hundreds of strong Bragg reflections that may offer a great number of choices for making fixed-angle X-ray analyzers and polarizers at virtually any hard X-ray energies with selectable resolution. However, quartz crystals, unlike silicon and germanium, are chiral and may thus appear in two different forms of handedness that are mirror images. Furthermore, because of the threefold rotational symmetry along thecaxis, the {h 1h 2h 3L} and {h 2h 1h 3L} Bragg reflections may have quite different Darwin bandwidth, reflectivity and angular acceptance, although they have the same Bragg angle. The design of X-ray optics from quartz crystalsmore » therefore requires unambiguous determination of the orientation, handedness and polarity of the crystals. The Laue method and single-axis diffraction technique can provide such information, but the variety of conventions used in the literature to describe quartz structures has caused widespread confusion. The current studies give detailed guidelines for design and fabrication of quartz X-ray optics, with special emphasis on the correct interpretation of Laue patterns in terms of the crystallography and diffraction properties of quartz. Meanwhile, the quartz crystals examined were confirmed by X-ray topography to have acceptably low densities of dislocations and other defects, which is the foundation for developing high-resolution quartz-based X-ray optics.« less

Studying the energy dependence of intrinsic conversion efficiency of single crystal scintillators under X-ray excitation

NASA Astrophysics Data System (ADS)

Kalyvas, N.; Valais, I.; David, S.; Michail, Ch.; Fountos, G.; Liaparinos, P.; Kandarakis, I.

2014-05-01

Single crystal scintilators are used in various radiation detectors applications. The efficiency of the crystal can be determined by the Detector Optical Gain (DOG) defined as the ratio of the emitted optical photon flux over the incident radiation photons flux. A parameter affecting DOG is the intrinsic conversion efficiency ( n C ) giving the percentage of the X-ray photon power converted to optical photon power. n C is considered a constant value for X-ray energies in the order of keV although a non-proportional behavior has been reported. In this work an analytical model, has been utilized to single crystals scintillators GSO:Ce, LSO:Ce and LYSO:Ce to examine whether the intrinsic conversion efficiency shows non proportional behavior under X-ray excitation. DOG was theoretically calculated as a function of the incident X-ray spectrum, the X-ray absorption efficiency, the energy of the produced optical photons and the light transmission efficiency. The theoretical DOG values were compared with experimental data obtained by irradiating the crystals with X-rays at tube voltages from 50 to 140 kV and by measuring the light energy flux emitted from the irradiated screen. An initial value for n C (calculated from literature data) was assumed for the X-ray tube voltage of 50 kV. For higher X-ray tube voltages the optical photon propagation phenomena was assumed constant and any deviations between experimental and theoretical data were associated with changes in the intrinsic conversion efficiency. The experimental errors were below 7% for each experimental setup. The behavior of n C values for LSO:Ce and LYSO:Ce were found very similar, i.e., ranging with values from 0.089 at 50 kV to 0.015 at 140 kV, while for GSO:Ce, n C demonstrated a peak at 80 kV.

Strain distribution in an Si single crystal measured by interference fringes of X-ray mirage diffraction

PubMed Central

Jongsukswat, Sukswat; Fukamachi, Tomoe; Ju, Dongying; Negishi, Riichirou; Hirano, Keiichi; Kawamura, Takaaki

2013-01-01

In X-ray interference fringes accompanied by mirage diffraction, variations have been observed in the spacing and position of the fringes from a plane-parallel Si single crystal fixed at one end as a function of distance from the incident plane of the X-rays to the free crystal end. The variations can be explained by distortion of the sample crystal due to gravity. From the variations and positions of the fringes, the strain gradient of the crystal has been determined. The distribution of the observed strain agrees with that expected from rod theory except for residual strain. When the distortion is large, the observed strain distribution does not agree with that expected from rod theory. PMID:24068841

Research of X-ray curved crystals analyzer

NASA Astrophysics Data System (ADS)

Xiao, Shali; Xong, Xian-cai; Qian, Jia-yu; Zhong, Xian-xin; Yan, Guo-hong; Liu, Zhong-li; Ding, Yong-kun

2005-08-01

X-ray spectrograph has long been used as a means of diagnosing conditions of laser-produced plasmas, as information concerning both the temperature and density can be extracted from the emitted radiation. For the measurement of X-ray lines in the energy range of 0.6-6 keV, A curved crystal X-ray spectrometer of reflection type elliptical geometry is required. In order to obtain both high resolution and collection efficiency the elliptical geometry is more advantageous than the flat configurations. Elliptical curved crystals spectrograph with a relatively wide spectral range are of particular use for deducing electron temperatures by measurement of the ratios of lines associated with different charge states. Curved crystals analyzer was designed and manufactured for use on an experiment to investigate the properties of laser produced plasmas. The spectrograph has 1350mm focal length and for these measurements, utilized PET, LIF, KAP and MICA crystal bent onto an elliptical substrate. This crystal analyzer covers the Bragg angel range from 30 to 67.5. The analyzer based on elliptically geometrical principle, which has self-focusing characteristics. The experiment was carried out on Shanghai Shengguang-II Facility and aimed to investigate the characteristics of a high density plasma. Experimental results using Curved crystal analyzer are described which show spectrum of Ti, Au laser-plasma. The focusing crystal analyzer clearly gave an increase in sensitivity over a flat crystal. Spectra showing the main resonance line were recorded with X-ray CCD and with laser energies 150J laser wavelength 350nm. The calculated wavelength resolution is about 500-1000.

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

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

DOE PAGES

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

2015-06-27

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

Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals

DOE PAGES

Dao, E. Han; Sierra, Raymond G.; Laksmono, Hartawan; ...

2015-04-30

In this work, we collected radiation-damage-free data from a set of cryo-cooled crystals for a novel 30S ribosomal subunit mutant using goniometer-based femtosecond crystallography. Crystal quality assessment for these samples was conducted at the X-ray Pump Probe end-station of the Linac Coherent Light Source (LCLS) using recently introduced goniometer-based instrumentation. These 30S subunit crystals were genetically engineered to omit a 26-residue protein, Thx, which is present in the wild-type Thermus thermophilus 30S ribosomal subunit. We are primarily interested in elucidating the contribution of this ribosomal protein to the overall 30S subunit structure. To assess the viability of this study, femtosecondmore » X-ray diffraction patterns from these crystals were recorded at the LCLS during a protein crystal screening beam time. During our data collection, we successfully observed diffraction from these difficult-to-grow 30S ribosomal subunit crystals. Most of our crystals were found to diffract to low resolution, while one crystal diffracted to 3.2 Å resolution. These data suggest the feasibility of pursuing high-resolution data collection as well as the need to improve sample preparation and handling in order to collect a complete radiation-damage-free data set using an X-ray Free Electron Laser.« less

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

PubMed

Tang, M X; Zhang, Y Y; E, J C; Luo, S N

2018-05-01

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

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

Tang, M. X.; Zhang, Y. Y.; E, J. C.

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of themore » diffraction patterns is discussed.« less

X-ray Crystallography Facility

NASA Technical Reports Server (NTRS)

1999-01-01

University of Alabama engineer Lance Weiss briefs NASA astronaut Dr. Bornie Dunbar about the design and capabilities of the X-ray Crystallography Facility under development at the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, AL, April 21, 1999. The X-ray Crystallography Facility is designed to speed the collection of protein structure information from crystals grown aboard the International Space Station. By measuring and mapping the protein crystal structure in space, researchers will avoid exposing the delicate crystals to the rigors of space travel and make important research data available to scientists much faster. The X-ray Crystallography facility is being designed and developed by the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, a NASA Commercial Space Center.

X-ray Crystallography Facility

NASA Technical Reports Server (NTRS)

1999-01-01

University of Alabama engineer Stacey Giles briefs NASA astronaut Dr. Bornie Dunbar about the design and capabilities of the X-ray Crystallography Facility under development at the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, AL, April 21, 1999. The X-ray Crystallography Facility is designed to speed the collection of protein structure information from crystals grown aboard the International Space Station. By measuring and mapping the protein crystal structure in space, researchers will avoid exposing the delicate crystals to the rigors of space travel and make important research data available to scientists much faster. The X-ray Crystallography facility is being designed and developed by the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, a NASA Commercial Space Center.

From Relativistic Electrons to X-ray Phase Contrast Imaging

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

Lumpkin, A. H.; Garson, A. B.; Anastasio, M. A.

2017-10-09

We report the initial demonstrations of the use of single crystals in indirect x-ray imaging for x-ray phase contrast imaging at the Washington University in St. Louis Computational Bioimaging Laboratory (CBL). Based on single Gaussian peak fits to the x-ray images, we observed a four times smaller system point spread function (21 μm (FWHM)) with the 25-mm diameter single crystals than the reference polycrystalline phosphor’s 80-μm value. Potential fiber-optic plate depth-of-focus aspects and 33-μm diameter carbon fiber imaging are also addressed.

Crystal structure and density of helium to 232 kbar

NASA Technical Reports Server (NTRS)

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

1988-01-01

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

X-ray spectrometer having 12 000 resolving power at 8 keV energy

NASA Astrophysics Data System (ADS)

Seely, John F.; Hudson, Lawrence T.; Henins, Albert; Feldman, Uri

2017-10-01

An x-ray spectrometer employing a thin (50 μm) silicon transmission crystal was used to record high-resolution Cu Kα spectra from a laboratory x-ray source. The diffraction was from the (331) planes that were at an angle of 13.26° to the crystal surface. The components of the spectral lines resulting from single-vacancy (1s) and double-vacancy (1s and 3d) transitions were observed. After accounting for the natural lifetime widths from reference double-crystal spectra and the spatial resolution of the image plate detector, the intrinsic broadening of the transmission crystal was measured to be as small as 0.67 eV and the resolving power 12 000, the highest resolving power achieved by a compact (0.5 m long) spectrometer employing a single transmission crystal operating in the hard x-ray region. By recording spectra with variable source-to-crystal distances and comparing to the calculated widths from various geometrical broadening mechanisms, the primary contributions to the intrinsic crystal broadening were found to be the source height at small distances and the crystal apertured height at large distances. By reducing these two effects, using a smaller source size and vignetting the crystal height, the intrinsic crystal broadening is then limited by the crystal thickness and the rocking curve width and would be 0.4 eV at 8 keV energy (20 000 resolving power).

p-type zinc-blende GaN on GaAs substrates

NASA Astrophysics Data System (ADS)

Lin, M. E.; Xue, G.; Zhou, G. L.; Greene, J. E.; Morkoç, H.

1993-08-01

We report p-type cubic GaN. The Mg-doped layers were grown on vicinal (100) GaAs substrates by plasma-enhanced molecular beam epitaxy. Thermally sublimed Mg was, with N2 carrier gas, fed into an electron-cyclotron resonance source. p-type zinc-blende-structure GaN films were achieved with hole mobilities as high as 39 cm2/V s at room temperature. The cubic nature of the films were confirmed by x-ray diffractometry. The depth profile of Mg was investigated by secondary ions mass spectroscopy.

Thermally Stable Nanocrystalline Steel

NASA Astrophysics Data System (ADS)

Hulme-Smith, Christopher Neil; Ooi, Shgh Woei; Bhadeshia, Harshad K. D. H.

2017-10-01

Two novel nanocrystalline steels were designed to withstand elevated temperatures without catastrophic microstructural changes. In the most successful alloy, a large quantity of nickel was added to stabilize austenite and allow a reduction in the carbon content. A 50 kg cast of the novel alloy was produced and used to verify the formation of nanocrystalline bainite. Synchrotron X-ray diffractometry using in situ heating showed that austenite was able to survive more than 1 hour at 773 K (500 °C) and subsequent cooling to ambient temperature. This is the first reported nanocrystalline steel with high-temperature capability.

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

Petrova, V. A.; Orekhov, A. S.; Chernyakov, D. D.

A method for preparing multilayer film composites based on chitosan has been developed by the example of polymer pairs: chitosan–hyaluronic acid, chitosan–alginic acid, and chitosan–carrageenan. The structure of the composite films is characterized by X-ray diffractometry and scanning electron microscopy. It is shown that the deposition of a solution of hyaluronic acid, alginic acid, or carrageenan on a chitosan gel film leads to the formation of a polyelectrolyte complex layer at the interface, which is accompanied by the ordering of chitosan chains in the surface region; the microstructure of this layer depends on the nature of contacting polymer pairs.

X-ray driven channeling acceleration in crystals and carbon nanotubes

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

Shin, Young-Min; Still, Dean A.; Shiltsev, Vladimir

2013-12-01

Acceleration of particles channeling in a crystal by means of diffracted x-rays via Bormann anomalous transmission was conceived for heavy ions and muons by Tajima and Cavenago [Phys. Rev. Lett. 59, 1440 (1987)], which potentially offers an appreciably high field gradient on the order of GV/cm. The theoretical model of the high gradient acceleration has been studied in two kinds of atomic structure, crystals and carbon nanotubes (CNTs), with analytic calculations and electromagnetic eigenmode simulations. A range of acceleration gradients and cutoffs of the x-ray power (the lowest power limit to overcome the Bremsstrahlung radiation losses) are characterized in termsmore » of the lattice constants, unit cell sizes, and photon energies. The parametric analysis indicates that the required x-ray power can be reduced to an order of megawatt by replacing crystals with CNTs. Eventually, the equivalent dielectric approximation of a multi-wall nanotube shows that 250–810 MeV muons can be synchronously coupled with x-rays of 0.65–1.32 keV in the accelerating structure.« less

Effects of fines content on hydraulic conductivity and morphology of laterite soil as hydraulic barrier

NASA Astrophysics Data System (ADS)

Bello Yamusa, Yamusa; Yunus, Nor Zurairahetty Mohd; Ahmad, Kamarudin; Rahman, Norhan Abd; Sa'ari, Radzuan

2018-03-01

Laterite soil was investigated to find out the effects of fines content and to identify the micro-structural and molecular characteristics to evaluate its potentiality as a compacted soil landfill liner material. Tests were carried out on natural soil and reconstituted soil by dry weight of soil samples to determine the physical and engineering properties of the soil. All tests were carried out on the samples by adopting the British Standard 1377:1990. The possible mechanisms that contributed to the clay mineralogy were analyzed using spectroscopic and microscopic techniques such as field emission scanning electron microscopy (FESEM), energy-dispersive X-ray (EDX) and X-ray diffractometry (XRD). The laterite soil was found to contain kaolinite as the major clay minerals. A minimum of 50% fines content of laterite soil met the required result for hydraulic barriers in waste containment facilities.

Observing Graphene Grow: Catalyst–Graphene Interactions during Scalable Graphene Growth on Polycrystalline Copper

PubMed Central

2013-01-01

Complementary in situ X-ray photoelectron spectroscopy (XPS), X-ray diffractometry, and environmental scanning electron microscopy are used to fingerprint the entire graphene chemical vapor deposition process on technologically important polycrystalline Cu catalysts to address the current lack of understanding of the underlying fundamental growth mechanisms and catalyst interactions. Graphene forms directly on metallic Cu during the high-temperature hydrocarbon exposure, whereby an upshift in the binding energies of the corresponding C1s XPS core level signatures is indicative of coupling between the Cu catalyst and the growing graphene. Minor carbon uptake into Cu can under certain conditions manifest itself as carbon precipitation upon cooling. Postgrowth, ambient air exposure even at room temperature decouples the graphene from Cu by (reversible) oxygen intercalation. The importance of these dynamic interactions is discussed for graphene growth, processing, and device integration. PMID:24041311

The ceramics of Malpaís of Zacapu, Michoacán, Mexico, during the Early and Middle Postclassic periods (900-1450 AD): Micro-chemical characterization of surface paintings

NASA Astrophysics Data System (ADS)

Jadot, E.; Schiavon, N.; Manso, M.

2016-05-01

Tarascan ceramic sherds from two Postclassical archaeological sites (900-1450 AD) at the Malpaís of Zacapu, Michoacán, Mexico, were investigated by combining Back-Scattered Scanning Electron Microscopy and Energy Dispersive Spectroscopy (BSEM-EDS), μ-X-Ray Diffractometry (μ-XRD), μ-X-ray Fluorescence Spectroscopy (μ-XRF) and μ-Raman Spectroscopy. These sherds are famous for their forms and decorations although the composition of its raw materials remains so far unknown and focused only on the composition of the ceramic paste. For the purpose of surface decoration characterization, the pigments used in slips and paintings were identified as hematite, magnetite, amorphous carbon, graphite and lignite. Furthermore chemical and molecular structure determination allowed the identification of technological aspects such as the firing temperatures and atmospheres used in ceramics production.

Hydrothermal epitaxy and resultant properties of EuTiO3 films on SrTiO3(001) substrate

PubMed Central

2014-01-01

We report a novel epitaxial growth of EuTiO3 films on SrTiO3(001) substrate by hydrothermal method. The morphological, structural, chemical, and magnetic properties of these epitaxial EuTiO3 films were examined by scanning electron microscopy, transmission electron microscopy, high-resolution X-ray diffractometry, X-ray photoelectron spectroscopy, and superconducting quantum interference device magnetometry, respectively. As-grown EuTiO3 films with a perovskite structure were found to show an out-of-plane lattice shrinkage and room-temperature ferromagnetism, possibly resulting from an existence of Eu3+. Postannealing at 1,000°C could reduce the amount of Eu3+, relax the out-of-plane lattice shrinkage, and impact the magnetic properties of the films. PACS 81.10.Aj; 81.15.-z; 61.05.-a PMID:24948889

Identifying, studying and making good use of macromolecular crystals

PubMed Central

Calero, Guillermo; Cohen, Aina E.; Luft, Joseph R.; Newman, Janet; Snell, Edward H.

2014-01-01

Structural biology has contributed tremendous knowledge to the understanding of life on the molecular scale. The Protein Data Bank, a depository of this structural knowledge, currently contains over 100 000 protein structures, with the majority stemming from X-ray crystallography. As the name might suggest, crystallography requires crystals. As detectors become more sensitive and X-ray sources more intense, the notion of a crystal is gradually changing from one large enough to embellish expensive jewellery to objects that have external dimensions of the order of the wavelength of visible light. Identifying these crystals is a prerequisite to their study. This paper discusses developments in identifying these crystals during crystallization screening and distinguishing them from other potential outcomes. The practical aspects of ensuring that once a crystal is identified it can then be positioned in the X-ray beam for data collection are also addressed. PMID:25084371

Solid state parameters, structure elucidation, High Resolution X-Ray Diffraction (HRXRD), phase matching, thermal and impedance analysis on L-Proline trichloroacetate (L-PTCA) NLO single crystals.

PubMed

Kalaiselvi, P; Raj, S Alfred Cecil; Jagannathan, K; Vijayan, N; Bhagavannarayana, G; Kalainathan, S

2014-11-11

Nonlinear optical single crystal of L-Proline trichloroacetate (L-PTCA) was successfully grown by Slow Evaporation Solution Technique (SEST). The grown crystals were subjected to single crystal X-ray diffraction analysis to confirm the structure. From the single crystal XRD data, solid state parameters were determined for the grown crystal. The crystalline perfection has been evaluated using high resolution X-ray diffractometer. The frequencies of various functional groups were identified from FTIR spectral analysis. The percentage of transmittance was obtained from UV Visible spectral analysis. TGA-DSC measurements indicate the thermal stability of the crystal. The dielectric constant, dielectric loss and ac conductivity were measured by the impedance analyzer. The DC conductivity was calculated by the cole-cole plot method. Copyright © 2014 Elsevier B.V. All rights reserved.

Synchrotron X-ray reciprocal-space mapping, topography and diffraction resolution studies of macromolecular crystal quality.

PubMed

Boggon, T J; Helliwell, J R; Judge, R A; Olczak, A; Siddons, D P; Snell, E H; Stojanoff, V

2000-07-01

A comprehensive study of microgravity and ground-grown chicken egg-white lysozyme crystals is presented using synchrotron X-ray reciprocal-space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed reduced intrinsic mosaicities on average, but no differences in terms of strain over their ground-grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the ground-control case only a small volume of the crystal contributed to the intensity at the diffraction peak. The techniques prove to be highly complementary, with the reciprocal-space mapping providing a quantitative measure of the crystal mosaicity and strain (or variation in lattice spacing) and the topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out at the synchrotron.

Synchrotron X-Ray Reciprocal Space Mapping, Topography and Diffraction Resolution Studies of Macromolecular Crystal Quality

NASA Technical Reports Server (NTRS)

Boggon, T. J.; Helliwell, J. R.; Judge, Russell A.; Siddons, D. P.; Snell, Edward H.; Stojanoff, V.

2000-01-01

A comprehensive study of microgravity and ground grown chicken egg white lysozyme crystals is presented using synchrotron X-ray reciprocal space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed, on average, reduced intrinsic mosaicities but no differences in terms of stress over their earth grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the earth case at the diffraction peak only a small volume of the crystal contributed to the intensity. The techniques prove to be highly complementary with the reciprocal space mapping providing a quantitative measure of the crystal mosaicity and stress (or variation in lattice spacing) and topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out both at the synchrotron and in the laboratory.

Apollo-Soyuz pamphlet no. 2: X-rays, gamma-rays. [experimental design

NASA Technical Reports Server (NTRS)

Page, L. W.; From, T. P.

1977-01-01

The nature of high energy radiation and its penetration through earth's atmosphere is examined with emphasis on X-rays, gamma rays, and cosmic radiation and the instruments used in their detection. The history of radio astronomy and the capabilities of the Uhuru satellite are summarized. The ASTP soft X-ray experiment (MA-048) designed to study the spectra in the range from 0.1 to 10 keV and survey the background over a large section of the sky is described, as well as the determination of SMC C-1 as an X-ray pulsar. The crystal activation experiment (MA-151) used to measure the radioactive isotopes created by cosmic rays in crystals used for gamma ray detectors is also discussed.

Room-temperature serial crystallography using a kinetically optimized microfluidic device for protein crystallization and on-chip X-ray diffraction

PubMed Central

Heymann, Michael; Opthalage, Achini; Wierman, Jennifer L.; Akella, Sathish; Szebenyi, Doletha M. E.; Gruner, Sol M.; Fraden, Seth

2014-01-01

An emulsion-based serial crystallographic technology has been developed, in which nanolitre-sized droplets of protein solution are encapsulated in oil and stabilized by surfactant. Once the first crystal in a drop is nucleated, the small volume generates a negative feedback mechanism that lowers the supersaturation. This mechanism is exploited to produce one crystal per drop. Diffraction data are measured, one crystal at a time, from a series of room-temperature crystals stored on an X-ray semi-transparent microfluidic chip, and a 93% complete data set is obtained by merging single diffraction frames taken from different unoriented crystals. As proof of concept, the structure of glucose isomerase was solved to 2.1 Å, demonstrating the feasibility of high-throughput serial X-ray crystallography using synchrotron radiation. PMID:25295176

Exploration of New Principles in Spintronics Based on Topological Insulators (Option 1)

DTIC Science & Technology

2012-05-14

on the surface and found that our crystals are exceedingly homogeneous (Supplementary Information). The persistently narrow X - ray diffraction peaks...modified Bridgman method (see Supplementary Information for details). X - ray diffraction measurements indicated the monotonic shrinkage of a and c axis...and annealing at that temperature for 4 days. X - ray diffraction analyses confirmed that all the samples have the same crystal structure (R 3m

Single-crystal diamond refractive lens for focusing X-rays in two dimensions.

PubMed

Antipov, S; Baryshev, S V; Butler, J E; Antipova, O; Liu, Z; Stoupin, S

2016-01-01

The fabrication and performance evaluation of single-crystal diamond refractive X-ray lenses of which the surfaces are paraboloids of revolution for focusing X-rays in two dimensions simultaneously are reported. The lenses were manufactured using a femtosecond laser micromachining process and tested using X-ray synchrotron radiation. Such lenses were stacked together to form a standard compound refractive lens (CRL). Owing to the superior physical properties of the material, diamond CRLs could become indispensable wavefront-preserving primary focusing optics for X-ray free-electron lasers and the next-generation synchrotron storage rings. They can be used for highly efficient refocusing of the extremely bright X-ray sources for secondary optical schemes with limited aperture such as nanofocusing Fresnel zone plates and multilayer Laue lenses.

Single-crystal diamond refractive lens for focusing X-rays in two dimensions

PubMed Central

Antipov, S.; Baryshev, S. V.; Butler, J. E.; Antipova, O.; Liu, Z.; Stoupin, S.

2016-01-01

The fabrication and performance evaluation of single-crystal diamond refractive X-ray lenses of which the surfaces are paraboloids of revolution for focusing X-rays in two dimensions simultaneously are reported. The lenses were manufactured using a femtosecond laser micromachining process and tested using X-ray synchrotron radiation. Such lenses were stacked together to form a standard compound refractive lens (CRL). Owing to the superior physical properties of the material, diamond CRLs could become indispensable wavefront-preserving primary focusing optics for X-ray free-electron lasers and the next-generation synchrotron storage rings. They can be used for highly efficient refocusing of the extremely bright X-ray sources for secondary optical schemes with limited aperture such as nanofocusing Fresnel zone plates and multilayer Laue lenses. PMID:26698059

Single-crystal diamond refractive lens for focusing X-rays in two dimensions

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

Antipov, S.; Baryshev, Sergey; Butler, J. E.

2016-01-01

The fabrication and performance evaluation of single-crystal diamond refractive X-ray lenses of which the surfaces are paraboloids of revolution for focusing X-rays in two dimensions simultaneously are reported. The lenses were manufactured using a femtosecond laser micromachining process and tested using X-ray synchrotron radiation. Such lenses were stacked together to form a standard compound refractive lens (CRL). Owing to the superior physical properties of the material, diamond CRLs could become indispensable wavefront-preserving primary focusing optics for X-ray free-electron lasers and the next-generation synchrotron storage rings. They can be used for highly efficient refocusing of the extremely bright X-ray sources formore » secondary optical schemes with limited aperture such as nanofocusing Fresnel zone plates and multilayer Laue lenses.« less

Studies on the growth, structural, spectral and third-order nonlinear optical properties of ammonium 3-carboxy-4-hydroxy benzenesulfonate monohydrate single crystal.

PubMed

Silambarasan, A; Krishna Kumar, M; Thirunavukkarasu, A; Mohan Kumar, R; Umarani, P R

2015-01-25

An organic nonlinear optical bulk single crystal, Ammonium 3-carboxy-4-hydroxy benzenesulfonate monohydrate (ACHBS) was successfully grown by solution growth technique. Single crystal X-ray diffraction study confirms that, the grown crystal belongs to P21/c space group. Powder X-ray diffraction and high resolution X-ray diffraction analyses revealed the crystallinity of the grown crystal. Infrared spectral analysis showed the vibrational behavior of chemical bonds and its functional groups. The thermal stability and decomposition stages of the grown crystal were studied by TG-DTA analysis. UV-Visible transmittance studies showed the transparency region and cut-off wavelength of the grown crystal. The third-order nonlinear optical susceptibility of the grown crystal was estimated by Z-scan technique using He-Ne laser source. The mechanical property of the grown crystal was studied by using Vicker's microhardness test. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation and Analysis of RNA Crystals

NASA Technical Reports Server (NTRS)

Todd, Paul

2000-01-01

The crystallization of RiboNucleic Acids (RNA) was studied from the standpoint of mechanisms of crystal growth in three tasks: (1) preparation of high-quality crystals of oligonuclotides for X-ray diffraction, (2) finding pathways to the growth of high-quality crystals for X-ray diffraction and (3) investigation of mechanisms of action of inertial acceleration on crystal growth. In these tasks: (1) RNA crystals were prepared and studied by X-ray diffraction; (2) a pathway to high-quality crystals was discovered and characterized; a combination of kinetic and equilibrium factors could be optimized as described below; and (3) an interplay between purity and gravity was found in a combination of space and ground experiments with nucleic acids and proteins. Most significantly, the rate of concentration of precipitant and RNA can be controlled by membrane-based methods of water removal or by diffusion of multivalent cations across an interface stabilized by a membrane. Oligonucleotide solutions are electrokinetically stabilized colloids, and crystals can form by the controlled addition of multivalent cations.

Purification, crystallization and preliminary X-ray diffraction studies of N-acetylglucosamine-phosphate mutase from Candida albicans

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

Nishitani, Yuichi; Maruyama, Daisuke; Nonaka, Tsuyoshi

2006-04-01

Preliminary X-ray diffraction studies on N-acetylglucosamine-phosphate mutase from C. albicans are reported. N-acetylglucosamine-phosphate mutase (AGM1) is an essential enzyme in the synthesis of UDP-N-acetylglucosamine (UDP-GlcNAc) in eukaryotes and belongs to the α-d-phosphohexomutase superfamily. AGM1 from Candida albicans (CaAGM1) was purified and crystallized by the sitting-drop vapour-diffusion method. The crystals obtained belong to the primitive monoclinic space group P2{sub 1}, with unit-cell parameters a = 60.2, b = 130.2, c = 78.0 Å, β = 106.7°. The crystals diffract X-rays to beyond 1.8 Å resolution using synchrotron radiation.

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

NASA Astrophysics Data System (ADS)

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

2015-05-01

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

Ferric ion-assisted in situ synthesis of silver nanoplates on polydopamine-coated silk.

PubMed

Xiao, Jing; Zhang, Huihui; Mao, Cuiping; Wang, Ying; Wang, Ling; Lu, Zhisong

2016-10-01

In the present study, a ferric ion (Fe(3+))-assisted in situ synthesis approach was developed to grow silver (Ag) nanoplates on the polydopamine (PDA)-coated silk without the use of additional reductants. The essential role of Fe(3+) in the formation of Ag nanoplates is revealed by comparing the morphologies of Ag nanostructures prepared on the silk-coated PDA film with/without Fe(3+) doping. Scanning electron micrographs show that high-density Ag nanoplates could be synthesized in the reaction system containing 50μg/mL FeCl3 and 50mM AgNO3. The size of the Ag nanoplate could be tuned by adjusting the reaction duration. Based on the data, a mechanism involving the Fe(3+)-selected growth of Ag atoms along the certain crystal faces was proposed to explain the fabrication process. Transmission electron microscopy and X-ray diffractometry indicate that the Ag nanoplates possess good crystalline structures. Raman spectra demonstrate that the nanoplates could strongly enhance the Raman scattering of the PDA molecules. The Ag nanoplate-coated silk could be utilized as a flexible substrate for the development of surface-enhanced Raman scattering biosensors. Copyright © 2016 Elsevier Inc. All rights reserved.

Observation of defect-induced Photoresponse and charge carrier transport in single GeSe2 nanobelt devices

NASA Astrophysics Data System (ADS)

Mukherjee, Bablu; Tok, Eng Soon; Haur Sow, Chorng

2013-03-01

Single crystal GeSe2 nanobelts were grown using chemical vapor deposition techniques. Morphology of the nanostructures was characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD) and Raman spectroscopy. Electronic transport properties, impedance spectroscopy, photoconductive characteristics and temperature-dependent electrical resistivity measurements were carried out on individual GeSe2 nanobelt devices. The photosensitivity of single GeSe2 nanobelt (NB) devices was examined with two different excitation wavelengths of laser beams with photon energies above band gap and at sub-band gap of the NB. A maximum photoconductive gain 106 % was achieved at a wavelength of 808 nm. The magnitude of the photocurrent and response time of the individual GeSe2 NB device indicate that the photoresponse could be attributed to the presence of isolated mid band gap defect levels. Temperature dependent photocurrent measurements indicate the rough estimation of the energy levels for the defect states. Localized photostudy shows that the large photoresponse of the device primarily occurs at the metal-NB contact regions. Department of Physics, 2 Science Drive 3, National University of Singapore (NUS), Singapore 117542

LiMn2O4–yBryNanoparticles Synthesized by a Room Temperature Solid-State Coordination Method

PubMed Central

2009-01-01

LiMn2O4–yBrynanoparticles were synthesized successfully for the first time by a room temperature solid-state coordination method. X-ray diffractometry patterns indicated that the LiMn2O4–yBrypowders were well-crystallized pure spinel phase. Transmission electron microscopy images showed that the LiMn2O4–yBrypowders consisted of small and uniform nanosized particles. Synthesis conditions such as the calcination temperature and the content of Br−were investigated to optimize the ideal condition for preparing LiMn2O4–yBrywith the best electrochemical performances. The optimized synthesis condition was found in this work; the calcination temperature is 800 °C and the content of Br−is 0.05. The initial discharge capacity of LiMn2O3.95Br0.05obtained from the optimized synthesis condition was 134 mAh/g, which is far higher than that of pure LiMn2O4, indicating introduction of Br−in LiMn2O4is quite effective in improving the initial discharge capacity. PMID:20628635

X-ray free electron laser: opportunities for drug discovery.

PubMed

Cheng, Robert K Y; Abela, Rafael; Hennig, Michael

2017-11-08

Past decades have shown the impact of structural information derived from complexes of drug candidates with their protein targets to facilitate the discovery of safe and effective medicines. Despite recent developments in single particle cryo-electron microscopy, X-ray crystallography has been the main method to derive structural information. The unique properties of X-ray free electron laser (XFEL) with unmet peak brilliance and beam focus allow X-ray diffraction data recording and successful structure determination from smaller and weaker diffracting crystals shortening timelines in crystal optimization. To further capitalize on the XFEL advantage, innovations in crystal sample delivery for the X-ray experiment, data collection and processing methods are required. This development was a key contributor to serial crystallography allowing structure determination at room temperature yielding physiologically more relevant structures. Adding the time resolution provided by the femtosecond X-ray pulse will enable monitoring and capturing of dynamic processes of ligand binding and associated conformational changes with great impact to the design of candidate drug compounds. © 2017 The Author(s). Published by Portland Press Limited on behalf of the Biochemical Society.

Crystallization and X-ray diffraction of crystals formed in water-plasticized amorphous lactose.

PubMed

Jouppila, K; Kansikas, J; Roos, Y H

1998-01-01

Effects of storage time and relative humidity on crystallization and crystal forms produced from amorphous lactose were investigated. Crystallization was observed from time-dependent loss of sorbed water and increasing intensities of peaks in X-ray diffraction patterns. The rate of crystallization increased with increasing storage relative humidity. Lactose crystallized mainly as alpha-lactose monohydrate and anhydrous crystals with alpha- and beta-lactose in a molar ratio of 5:3. The results suggested that the crystal form was defined by the early nucleation process. The crystallization data are important in modeling of crystallization phenomena and prediction of stability of lactose-containing food and pharmaceutical materials.

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

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

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

A preliminary design study for a cosmic X-ray spectrometer

NASA Technical Reports Server (NTRS)

1972-01-01

The results are described of theoretical and experimental investigations aimed at the development of a curved crystal cosmic X-ray spectrometer to be used at the focal plane of the large orbiting X-ray telescope on the third High Energy Astronomical Observatory. The effort was concentrated on the development of spectrometer concepts and their evaluation by theoretical analysis, computer simulation, and laboratory testing with breadboard arrangements of crystals and detectors. In addition, a computer-controlled facility for precision testing and evaluation of crystals in air and vacuum was constructed. A summary of research objectives and results is included.

Crystals for astronomical X-ray spectroscopy

NASA Technical Reports Server (NTRS)

Burek, A.

1976-01-01

Crystal spectrometric properties and the factors that affect their measurement are discussed. Theoretical and experimental results on KAP are summarized and theoretical results based on the dynamical theory of X-ray diffraction are given for the acid phthalates as well as for the commonly used planes of ADP, PET and EDDT. Anomalous dispersion is found to be important for understanding the details of crystal Bragg reflection properties at long X-ray wavelengths and some important effects are pointed out. The theory of anomalous dispersion is applied to explain the anomalous reflectivity exhibited by KAP at 23.3 A.

X-Ray Topography of Tetragonal Lysozyme Grown by the Temperature-Controlled Technique

NASA Technical Reports Server (NTRS)

Stojanoff, V.; Siddons, D. P.; Monaco, Lisa A.; Vekilov, Peter; Rosenberger, Franz

1997-01-01

Growth-induced defects in lysozyme crystals were observed by white-beam and monochromatic X-ray topography at the National Synchrotron Light Source (NSLS) at the Brookhaven National Laboratory (BNL). The topographic methods were non-destructive to the extent that traditional diffraction data collection could be performed to high resolution after topography. It was found that changes in growth parameters, defect concentration as detected by X-ray topography, and the diffraction quality obtainable from the crystals were all strongly correlated. In addition, crystals with fewer defects showed lower mosaicity and higher diffraction resolution as expected.

A soft x-ray octadecyl hydrogen maleate crystal spectrograph

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

Fan, P.Z.; Fill, E.E.; Tietang, G.

1996-03-01

A crystal spectrograph is described which can be used to investigate laser-produced plasmas in the region of soft x rays at wavelengths of up to 60 A. The spectrograph uses an octadecyl hydrogen maleate crystal with a 2{ital d} of 63.5 A, combined with a very thin carbon filter (3000 A thick). As examples of its application, soft x-ray spectra in the range of 43{endash}51 A from laser plasmas of Si and Cu are presented. A spectral resolution of {lambda}/{Delta}{lambda}=1100 is deduced from the spectra. {copyright} {ital 1996 American Institute of Physics.}

Femtosecond X-ray protein nanocrystallography.

PubMed

Chapman, Henry N; Fromme, Petra; Barty, Anton; White, Thomas A; Kirian, Richard A; Aquila, Andrew; Hunter, Mark S; Schulz, Joachim; DePonte, Daniel P; Weierstall, Uwe; Doak, R Bruce; Maia, Filipe R N C; Martin, Andrew V; Schlichting, Ilme; Lomb, Lukas; Coppola, Nicola; Shoeman, Robert L; Epp, Sascha W; Hartmann, Robert; Rolles, Daniel; Rudenko, Artem; Foucar, Lutz; Kimmel, Nils; Weidenspointner, Georg; Holl, Peter; Liang, Mengning; Barthelmess, Miriam; Caleman, Carl; Boutet, Sébastien; Bogan, Michael J; Krzywinski, Jacek; Bostedt, Christoph; Bajt, Saša; Gumprecht, Lars; Rudek, Benedikt; Erk, Benjamin; Schmidt, Carlo; Hömke, André; Reich, Christian; Pietschner, Daniel; Strüder, Lothar; Hauser, Günter; Gorke, Hubert; Ullrich, Joachim; Herrmann, Sven; Schaller, Gerhard; Schopper, Florian; Soltau, Heike; Kühnel, Kai-Uwe; Messerschmidt, Marc; Bozek, John D; Hau-Riege, Stefan P; Frank, Matthias; Hampton, Christina Y; Sierra, Raymond G; Starodub, Dmitri; Williams, Garth J; Hajdu, Janos; Timneanu, Nicusor; Seibert, M Marvin; Andreasson, Jakob; Rocker, Andrea; Jönsson, Olof; Svenda, Martin; Stern, Stephan; Nass, Karol; Andritschke, Robert; Schröter, Claus-Dieter; Krasniqi, Faton; Bott, Mario; Schmidt, Kevin E; Wang, Xiaoyu; Grotjohann, Ingo; Holton, James M; Barends, Thomas R M; Neutze, Richard; Marchesini, Stefano; Fromme, Raimund; Schorb, Sebastian; Rupp, Daniela; Adolph, Marcus; Gorkhover, Tais; Andersson, Inger; Hirsemann, Helmut; Potdevin, Guillaume; Graafsma, Heinz; Nilsson, Björn; Spence, John C H

2011-02-03

X-ray crystallography provides the vast majority of macromolecular structures, but the success of the method relies on growing crystals of sufficient size. In conventional measurements, the necessary increase in X-ray dose to record data from crystals that are too small leads to extensive damage before a diffraction signal can be recorded. It is particularly challenging to obtain large, well-diffracting crystals of membrane proteins, for which fewer than 300 unique structures have been determined despite their importance in all living cells. Here we present a method for structure determination where single-crystal X-ray diffraction 'snapshots' are collected from a fully hydrated stream of nanocrystals using femtosecond pulses from a hard-X-ray free-electron laser, the Linac Coherent Light Source. We prove this concept with nanocrystals of photosystem I, one of the largest membrane protein complexes. More than 3,000,000 diffraction patterns were collected in this study, and a three-dimensional data set was assembled from individual photosystem I nanocrystals (∼200 nm to 2 μm in size). We mitigate the problem of radiation damage in crystallography by using pulses briefer than the timescale of most damage processes. This offers a new approach to structure determination of macromolecules that do not yield crystals of sufficient size for studies using conventional radiation sources or are particularly sensitive to radiation damage.

A split-beam probe-pump-probe scheme for femtosecond time resolved protein X-ray crystallography

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

van Thor, Jasper J.; Madsen, Anders

In order to exploit the femtosecond pulse duration of X-ray Free-Electron Lasers (XFEL) operating in the hard X-ray regime for ultrafast time-resolved protein crystallography experiments, critical parameters that determine the crystallographic signal-to-noise (I/σI) must be addressed. For single-crystal studies under low absorbed dose conditions, it has been shown that the intrinsic pulse intensity stability as well as mode structure and jitter of this structure, significantly affect the crystallographic signal-to-noise. Here, geometrical parameters are theoretically explored for a three-beam scheme: X-ray probe, optical pump, X-ray probe (or “probe-pump-probe”) which will allow experimental determination of the photo-induced structure factor amplitude differences, ΔF,more » in a ratiometric manner, thereby internally referencing the intensity noise of the XFEL source. In addition to a non-collinear split-beam geometry which separates un-pumped and pumped diffraction patterns on an area detector, applying an additional convergence angle to both beams by focusing leads to integration over mosaic blocks in the case of well-ordered stationary protein crystals. Ray-tracing X-ray diffraction simulations are performed for an example using photoactive yellow protein crystals in order to explore the geometrical design parameters which would be needed. The specifications for an X-ray split and delay instrument that implements both an offset angle and focused beams are discussed, for implementation of a probe-pump-probe scheme at the European XFEL. We discuss possible extension of single crystal studies to serial femtosecond crystallography, particularly in view of the expected X-ray damage and ablation due to the first probe pulse.« less

A split-beam probe-pump-probe scheme for femtosecond time resolved protein X-ray crystallography

DOE PAGES

van Thor, Jasper J.; Madsen, Anders

2015-01-01

In order to exploit the femtosecond pulse duration of X-ray Free-Electron Lasers (XFEL) operating in the hard X-ray regime for ultrafast time-resolved protein crystallography experiments, critical parameters that determine the crystallographic signal-to-noise (I/σI) must be addressed. For single-crystal studies under low absorbed dose conditions, it has been shown that the intrinsic pulse intensity stability as well as mode structure and jitter of this structure, significantly affect the crystallographic signal-to-noise. Here, geometrical parameters are theoretically explored for a three-beam scheme: X-ray probe, optical pump, X-ray probe (or “probe-pump-probe”) which will allow experimental determination of the photo-induced structure factor amplitude differences, ΔF,more » in a ratiometric manner, thereby internally referencing the intensity noise of the XFEL source. In addition to a non-collinear split-beam geometry which separates un-pumped and pumped diffraction patterns on an area detector, applying an additional convergence angle to both beams by focusing leads to integration over mosaic blocks in the case of well-ordered stationary protein crystals. Ray-tracing X-ray diffraction simulations are performed for an example using photoactive yellow protein crystals in order to explore the geometrical design parameters which would be needed. The specifications for an X-ray split and delay instrument that implements both an offset angle and focused beams are discussed, for implementation of a probe-pump-probe scheme at the European XFEL. We discuss possible extension of single crystal studies to serial femtosecond crystallography, particularly in view of the expected X-ray damage and ablation due to the first probe pulse.« less

A split-beam probe-pump-probe scheme for femtosecond time resolved protein X-ray crystallography

PubMed Central

van Thor, Jasper J.; Madsen, Anders

2015-01-01

In order to exploit the femtosecond pulse duration of X-ray Free-Electron Lasers (XFEL) operating in the hard X-ray regime for ultrafast time-resolved protein crystallography experiments, critical parameters that determine the crystallographic signal-to-noise (I/σI) must be addressed. For single-crystal studies under low absorbed dose conditions, it has been shown that the intrinsic pulse intensity stability as well as mode structure and jitter of this structure, significantly affect the crystallographic signal-to-noise. Here, geometrical parameters are theoretically explored for a three-beam scheme: X-ray probe, optical pump, X-ray probe (or “probe-pump-probe”) which will allow experimental determination of the photo-induced structure factor amplitude differences, ΔF, in a ratiometric manner, thereby internally referencing the intensity noise of the XFEL source. In addition to a non-collinear split-beam geometry which separates un-pumped and pumped diffraction patterns on an area detector, applying an additional convergence angle to both beams by focusing leads to integration over mosaic blocks in the case of well-ordered stationary protein crystals. Ray-tracing X-ray diffraction simulations are performed for an example using photoactive yellow protein crystals in order to explore the geometrical design parameters which would be needed. The specifications for an X-ray split and delay instrument that implements both an offset angle and focused beams are discussed, for implementation of a probe-pump-probe scheme at the European XFEL. We discuss possible extension of single crystal studies to serial femtosecond crystallography, particularly in view of the expected X-ray damage and ablation due to the first probe pulse. PMID:26798786

Quantitative Kα line spectroscopy for energy transport in ultra-intense laser plasma interaction

NASA Astrophysics Data System (ADS)

Zhang, Z.; Nishimura, H.; Namimoto, T.; Fujioka, S.; Arikawa, Y.; Nakai, M.; Koga, M.; Shiraga, H.; Kojima, S.; Azechi, H.; Ozaki, T.; Chen, H.; Pakr, J.; Williams, G. J.; Nishikino, M.; Kawachi, T.; Sagisaka, A.; Orimo, S.; Ogura, K.; Pirozhkov, A.; Yogo, A.; Kiriyama, H.; Kondo, K.; Okano, Y.

2012-10-01

X-ray line spectra ranging from 17 to 77 keV were quantitatively measured with a Laue spectrometer, composed of a cylindrically curved crystal and a detector. The absolute sensitivity of the spectrometer system was calibrated using pre-characterized laser-produced x-ray sources and radioisotopes, for the detectors and crystal respectively. The integrated reflectivity for the crystal is in good agreement with predictions by an open code for x-ray diffraction. The energy transfer efficiency from incident laser beams to hot electrons, as the energy transfer agency for Au Kα x-ray line emissions, is derived as a consequence of this work. By considering the hot electron temperature, the transfer efficiency from LFEX laser to Au plate target is about 8% to 10%.

Rapid soft X-ray fluctuations in solar flares observed with the X-ray polychromator

NASA Technical Reports Server (NTRS)

Zarro, D. M.; Saba, J. L. R.; Strong, K. T.

1986-01-01

Three flares observed by the Soft X-Ray Polychromator on the Solar Maximum Mission were studied. Flare light curves from the Flat Crystal Spectrometer and Bent Crystal Spectrometer were examined for rapid signal variations. Each flare was characterized by an initial fast (less than 1 min) burst, observed by the Hard X-Ray Burst Spectrometer (HXRBS), followed by softer gradual X-ray emission lasting several minutes. From an autocorrelation function analysis, evidence was found for quasi-periodic fluctuations with rise and decay times of 10 s in the Ca XIX and Fe XXV light curves. These variations were of small amplitude (less than 20%), often coincided with hard X-ray emissions, and were prominent during the onset of the gradual phase after the initial hard X-ray burst. It is speculated that these fluctuations were caused by repeated energy injections in a coronal loop that had already been heated and filled with dense plasma associated with the initial hard X-ray burst.

Capacity fading of LiAlyNi1-x-yCoxO2 cathode for lithium-ion batteries during accelerated calendar and cycle life tests (effect of depth of discharge in charge-discharge cycling on the suppression of the micro-crack generation of LiAlyNi1-x-yCoxO2 particle)

NASA Astrophysics Data System (ADS)

Watanabe, Shoichiro; Kinoshita, Masahiro; Hosokawa, Takashi; Morigaki, Kenichi; Nakura, Kensuke

2014-08-01

Cycle performance of a LiAl0.10Ni0.76Co0.14O2 (NCA) cathode/graphite cell closely depended on the range of depth of discharge in charge-discharge processes (ΔDOD). When ΔDOD was 10-70%, cycle performance at 25 °C was maintained even at 60 °C. Deterioration phenomena were analyzed by electrochemical method, X-ray photoelectron spectroscopy (XPS), X-ray diffractometry (XRD), and micro-cracks in NCA particles were analyzed with cross-sectional views by scanning electron microscopy (SEM). Many micro-cracks were observed only after a 0-100% DOD region cycle test. Cycle tests in several restricted ΔDOD conditions showed that the deterioration was closely related to not the upper and lower limits of DOD or operation voltage but the width of ΔDOD.

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

PubMed

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

2014-12-10

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

Applications of Coherent Radiation from Electrons traversing Crystals

NASA Astrophysics Data System (ADS)

Überall, H.

2000-04-01

Historically, the first types of coherent radiation from electrons traversing crystals studied were coherent bremsstrahlung (CB: Dyson and Überall 1955; Überall 1956, 1962) and channeling radiation (CR: Kumakhov, 1976) which produce quasimonochromatic X-rays and γ-rays, as well as parametric X-rays (Baryshevsky and Feranchuk, 1983). Related non-crystal sources are transition radiation and synchrotron radiation. We here present a comparison of radiation types from these sources, and we discuss a series of their possible applications, namely (a) CR: X-ray lithography, angiography, structure analysis of macromolecules, and trace element analysis, and (b) for CB: Radiography, use as a neutron source, elemental analysis, radiation therapy, and radioisotope production for commercial or medical use. CR and CB are very intense sources, needing only low-energy, moderately-priced electron linacs for their generation, hence competing with (or surpassing) more conventional X-ray sources intensity-wise and from a cost standpoint.

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

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

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

2014-04-24

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

Observing the overall rocking motion of a protein in a crystal

NASA Astrophysics Data System (ADS)

Ma, Peixiang; Xue, Yi; Coquelle, Nicolas; Haller, Jens D.; Yuwen, Tairan; Ayala, Isabel; Mikhailovskii, Oleg; Willbold, Dieter; Colletier, Jacques-Philippe; Skrynnikov, Nikolai R.; Schanda, Paul

2015-10-01

The large majority of three-dimensional structures of biological macromolecules have been determined by X-ray diffraction of crystalline samples. High-resolution structure determination crucially depends on the homogeneity of the protein crystal. Overall `rocking' motion of molecules in the crystal is expected to influence diffraction quality, and such motion may therefore affect the process of solving crystal structures. Yet, so far overall molecular motion has not directly been observed in protein crystals, and the timescale of such dynamics remains unclear. Here we use solid-state NMR, X-ray diffraction methods and μs-long molecular dynamics simulations to directly characterize the rigid-body motion of a protein in different crystal forms. For ubiquitin crystals investigated in this study we determine the range of possible correlation times of rocking motion, 0.1-100 μs. The amplitude of rocking varies from one crystal form to another and is correlated with the resolution obtainable in X-ray diffraction experiments.

Rapid disintegrating tablets of simvastatin dispersions in polyoxyethylene–polypropylene block copolymer for maximized disintegration and dissolution

PubMed Central

Balata, Gehan F; Zidan, Ahmad S; Abourehab, Mohamad AS; Essa, Ebtessam A

2016-01-01

The objective of this research was to improve the dissolution of simvastatin and to incorporate it in rapid disintegrating tablets (RDTs) with an optimized disintegration and dissolution characteristics. Polyoxyethylene–polypropylene block copolymer (poloxamer 188) was employed as a hydrophilic carrier to prepare simvastatin solid dispersions (SDs). Fourier transform infrared spectroscopy, differential scanning calorimetry (DSC) and X-ray diffractometry were employed to understand the interaction between the drug and the carrier in the solid state. The results obtained from Fourier transform infrared spectroscopy showed absence of any chemical interaction between the drug and poloxamer. The results of differential scanning calorimetry and X-ray diffractometry confirmed the conversion of simvastatin to distorted crystalline state. The SD of 1:2 w/w drug to carrier ratio showed the highest dissolution; hence, it was incorporated in RDT formulations using a 32 full factorial design and response surface methodology. The initial assessments of RDTs demonstrated an acceptable flow, hardness, and friability to indicate good mechanical strength. The interaction and Pareto charts indicated that percentage of croscarmellose sodium incorporated was the most important factor affecting the disintegration time and dissolution parameter followed by the hardness value and their interaction effect. Compression force showed a superior influence to increase RDT’s porosity and to fasten disintegration rather than swelling action by croscarmellose sodium. On the other hand, croscarmellose sodium was most important for the initial simvastatin release. The results suggest the potential use of poloxamer 188-based SD in RDT for the oral delivery of poor water-soluble antihyperlipidemic drug, simvastatin. PMID:27757012

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

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

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

2016-05-23

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

Method of Generating X-Ray Diffraction Data for Integral Detection of Twin Defects in Super-Hetero-Epitaxial Materials

NASA Technical Reports Server (NTRS)

Park, Yeonjoon (Inventor); Choi, Sang Hyouk (Inventor); King, Glen C. (Inventor); Elliott, James R. (Inventor)

2009-01-01

A method provides X-ray diffraction (XRD) data suitable for integral detection of a twin defect in a strained or lattice-matched epitaxial material made from components having crystal structures having symme try belonging to different space groups. The material is mounted in a n X-ray diffraction (XRD) system. In one embodiment, the XRD system's goniometer angle Omega is set equal to (Theta(sub B)-Beta) where The ta(sub B) is a Bragg angle for a designated crystal plane of the allo y that is disposed at a non-perpendicular orientation with respect to the {111) crystal plane, and Beta is the angle between the designate d crystal plane and a { 111 } crystal plane of one of the epitaxial components. The XRD system's detector angle is set equal to (Theta(su b B)+Beta). The material can be rotated through an angle of azimuthal rotation Phi about the axis aligned with the material. Using the det ector, the intensity of the X-ray diffraction is recorded at least at the angle at which the twin defect occurs.

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

PubMed

Tsujino, Soichiro; Tomizaki, Takashi

2016-05-06

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

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

NASA Astrophysics Data System (ADS)

Tsujino, Soichiro; Tomizaki, Takashi

2016-05-01

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

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

PubMed Central

Tsujino, Soichiro; Tomizaki, Takashi

2016-01-01

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

Experimental and theoretical investigation of the rocking curves measured for Mo K α X-ray characteristic lines in the double-crystal nondispersive scheme

NASA Astrophysics Data System (ADS)

Marchenkov, N. V.; Chukhovskii, F. N.; Blagov, A. E.

2015-03-01

The rocking curves (RCs) for Mo K α1 h Mo K α2 characteristic X-ray lines have been experimentally and theoretically studied in the nondispersive scheme of an X-ray double-crystal TPC-K diffractometer. The results of measurements and theoretical calculations of double-crystal RCs for characteristic X-rays from tubes with a molybdenum anode and different widths of slits show that a decrease in the slit width leads to an increase in the relative contribution of the Mo K α2-line RC in comparison with the intensity of the tails of the Mo K α1-line RC. It is shown that the second peak of the Mo K α2 line becomes increasingly pronounced in the tail of the Mo K α1-line RC with a decrease in the slit width. Two plane-parallel Si plates (input faces {110}, diffraction vector h <220>) were used as a monochromator crystal and a sample. The results of measuring double-crystal RCs are in good agreement with theoretical calculations.

Monochromatic X-ray sources based on a mechanism of real and virtual photon diffraction in crystals

NASA Astrophysics Data System (ADS)

Wagner, A. R.; Kuznetsov, S. I.; Potylitsyn, A. P.; Razin, S. V.; Uglov, S. R.; Zabaev, V. N.

2008-09-01

A source of monochromatic X-ray radiation is wanted in industry, science, medicine and so on. Many ways of making such a source are known. The present work describes two mechanisms for the creation of a monochromatic X-ray beam, which are parametric X-ray radiation (PXR) and bremsstrahlung diffraction (DBS). Both the experiments were carried out using an electron beam at a microtron. During the first experiment, the DBS process was investigated as a scattering of the Bremsstrahlung (BS) beam on the crystallographic surfaces of tungsten and pyrolytic graphite crystals. The second experiment consisted in the registration of the PXR and DBS yield during the passage of the electrons through the same crystals as in the first experiment. The spectral and orientation radiation characteristics and simulation results obtained for the DBS and PXR processes are presented. It is shown that the usage of mosaic crystalline targets is rather useful in order to obtain a monochromatic X-ray source based on bremsstrahlung diffraction from moderately relativistic electrons.

Acoustic Injectors for Drop-On-Demand Serial Femtosecond Crystallography

DOE PAGES

Roessler, Christian G.; Agarwal, Rakhi; Allaire, Marc; ...

2016-03-17

X-ray free-electron lasers (XFELs) provide very intense X-ray pulses suitable for macromolecular crystallography. Each X-ray pulse typically lasts for tens of femtoseconds and the interval between pulses is many orders of magnitude longer. Here we describe two novel acoustic injection systems that use focused sound waves to eject picoliter to nanoliter crystal-containing droplets out of microplates and into the X-ray pulse from which diffraction data are collected. The on-demand droplet delivery is synchronized to the XFEL pulse scheme, resulting in X-ray pulses intersecting up to 88% of the droplets. We tested several types of samples in a range of crystallizationmore » conditions, wherein the overall crystal hit ratio (e.g., fraction of images with observable diffraction patterns) is a function of the microcrystal slurry concentration. Lastly, we report crystal structures from lysozyme, thermolysin, and stachydrine demethylase (Stc2). In addition, samples were screened to demonstrate that these methods can be applied to rare samples« less

Acoustic Injectors for Drop-On-Demand Serial Femtosecond Crystallography

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

Roessler, Christian G.; Agarwal, Rakhi; Allaire, Marc

X-ray free-electron lasers (XFELs) provide very intense X-ray pulses suitable for macromolecular crystallography. Each X-ray pulse typically lasts for tens of femtoseconds and the interval between pulses is many orders of magnitude longer. Here we describe two novel acoustic injection systems that use focused sound waves to eject picoliter to nanoliter crystal-containing droplets out of microplates and into the X-ray pulse from which diffraction data are collected. The on-demand droplet delivery is synchronized to the XFEL pulse scheme, resulting in X-ray pulses intersecting up to 88% of the droplets. We tested several types of samples in a range of crystallizationmore » conditions, wherein the overall crystal hit ratio (e.g., fraction of images with observable diffraction patterns) is a function of the microcrystal slurry concentration. We report crystal structures from lysozyme, thermolysin, and stachydrine demethylase (Stc2). Additional samples were screened to demonstrate that these methods can be applied to rare samples.« less

Acoustic Injectors for Drop-On-Demand Serial Femtosecond Crystallography

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

Roessler, Christian G.; Agarwal, Rakhi; Allaire, Marc

X-ray free-electron lasers (XFELs) provide very intense X-ray pulses suitable for macromolecular crystallography. Each X-ray pulse typically lasts for tens of femtoseconds and the interval between pulses is many orders of magnitude longer. Here we describe two novel acoustic injection systems that use focused sound waves to eject picoliter to nanoliter crystal-containing droplets out of microplates and into the X-ray pulse from which diffraction data are collected. The on-demand droplet delivery is synchronized to the XFEL pulse scheme, resulting in X-ray pulses intersecting up to 88% of the droplets. We tested several types of samples in a range of crystallizationmore » conditions, wherein the overall crystal hit ratio (e.g., fraction of images with observable diffraction patterns) is a function of the microcrystal slurry concentration. Lastly, we report crystal structures from lysozyme, thermolysin, and stachydrine demethylase (Stc2). In addition, samples were screened to demonstrate that these methods can be applied to rare samples« less

X-ray-generated heralded macroscopical quantum entanglement of two nuclear ensembles.

PubMed

Liao, Wen-Te; Keitel, Christoph H; Pálffy, Adriana

2016-09-19

Heralded entanglement between macroscopical samples is an important resource for present quantum technology protocols, allowing quantum communication over large distances. In such protocols, optical photons are typically used as information and entanglement carriers between macroscopic quantum memories placed in remote locations. Here we investigate theoretically a new implementation which employs more robust x-ray quanta to generate heralded entanglement between two crystal-hosted macroscopical nuclear ensembles. Mössbauer nuclei in the two crystals interact collectively with an x-ray spontaneous parametric down conversion photon that generates heralded macroscopical entanglement with coherence times of approximately 100 ns at room temperature. The quantum phase between the entangled crystals can be conveniently manipulated by magnetic field rotations at the samples. The inherent long nuclear coherence times allow also for mechanical manipulations of the samples, for instance to check the stability of entanglement in the x-ray setup. Our results pave the way for first quantum communication protocols that use x-ray qubits.

A phase-contrast X-ray imaging system—with a 60×30 mm field of view—based on a skew-symmetric two-crystal X-ray interferometer

NASA Astrophysics Data System (ADS)

Yoneyama, Akio; Takeda, Tohoru; Tsuchiya, Yoshinori; Wu, Jin; Thet-Thet-Lwin; Koizumi, Aritaka; Hyodo, Kazuyuki; Itai, Yuji

2004-05-01

A phase-contrast X-ray imaging system—with a 60×30 mm field of view—for biomedical observations was developed. To extend the observation field of view, the system is fitted with a skew-symmetric two-crystal X-ray interferometer. To attain the required sub-nanoradian mechanical stability between the crystal blocks for precise operation, the interferometer was mounted on two extremely rigid positioning tables (one with a sleeve bearings) and was controlled by a feedback positioning system using phase-lock interferometry. The imaging system produced a 60×30 mm interference pattern with 60% visibility using 17.7 keV monochromatic synchrotron X-rays at the Photon Factory. It was then used to perform radiographic observation (i.e., phase mapping) of rat liver vessels. These results indicate that this imaging system can be used to perform observations of large and in vivo biological samples.

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

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

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 amore » 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.« less

Spatial resolution of a spherical x-ray crystal spectrometer at various magnifications

DOE PAGES

Gao, Lan; Hill, K. W.; Bitter, M.; ...

2016-08-23

Here, a high spatial resolution of a few μm is often required for probing small-scale high-energy-density plasmas using high resolution x-ray imaging spectroscopy. This resolution can be achieved by adjusting system magnification to overcome the inherent limitation of the detector pixel size. Laboratory experiments on investigating the relation between spatial resolution and system magnification for a spherical crystal spectrometer are presented. Tungsten Lβ 2 rays from a tungsten-target micro-focus x-ray tube were diffracted by a Ge 440 crystal, which was spherically bent to a radius of 223 mm, and imaged onto an x-ray CCD with 13-μm pixel size. The source-to-crystalmore » (p) and crystal-to-detector (q) distances were varied to produce spatial magnifications ( M = q/p) ranging from 2 to 10. The inferred instrumental spatial width reduces with increasing system magnification M. However, the experimental measurement at each M is larger than the theoretical value of pixel size divided by M. Future work will focus on investigating possible broadening mechanisms that limit the spatial resolution.« less

Laboratory-based micro-X-ray fluorescence setup using a von Hamos crystal spectrometer and a focused beam X-ray tube

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

Kayser, Y., E-mail: yves.kayser@psi.ch; Paul Scherrer Institut, 5232 Villigen-PSI; Błachucki, W.

2014-04-15

The high-resolution von Hamos bent crystal spectrometer of the University of Fribourg was upgraded with a focused X-ray beam source with the aim of performing micro-sized X-ray fluorescence (XRF) measurements in the laboratory. The focused X-ray beam source integrates a collimating optics mounted on a low-power micro-spot X-ray tube and a focusing polycapillary half-lens placed in front of the sample. The performances of the setup were probed in terms of spatial and energy resolution. In particular, the fluorescence intensity and energy resolution of the von Hamos spectrometer equipped with the novel micro-focused X-ray source and a standard high-power water-cooled X-raymore » tube were compared. The XRF analysis capability of the new setup was assessed by measuring the dopant distribution within the core of Er-doped SiO{sub 2} optical fibers.« less

Calorimetric and Diffractometric Evidence for the Sequential Crystallization of Buffer Components and the Consequential pH Swing in Frozen Solutions

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

Sundaramurthi, Prakash; Shalaev, Evgenyi; Suryanarayanan, Raj

2010-06-22

Sequential crystallization of succinate buffer components in the frozen solution has been studied by differential scanning calorimetry and X-ray diffractometry (both laboratory and synchrotron sources). The consequential pH shifts were monitored using a low-temperature electrode. When a solution buffered to pH < pK{sub a2} was cooled from room temperature (RT), the freeze-concentrate pH first increased and then decreased. This was attributed to the sequential crystallization of succinic acid, monosodium succinate, and finally disodium succinate. When buffered to pH > pK{sub a2}, the freeze-concentrate pH first decreased and then increased due to the sequential crystallization of the basic (disodium succinate) followedmore » by the acidic (monosodium succinate and succinic acid) buffer components. XRD provided direct evidence of the crystallization events in the frozen buffer solutions, including the formation of disodium succinate hexahydrate [Na{sub 2}(CH{sub 2}COO){sub 2} {center_dot} 6H{sub 2}O]. When the frozen solution was warmed in a differential scanning calorimeter, multiple endotherms attributable to the melting of buffer components and ice were observed. When the frozen solutions were dried under reduced pressure, ice sublimation was followed by dehydration of the crystalline hexahydrate to a poorly crystalline anhydrate. However, crystalline succinic acid and monosodium succinate were retained in the final lyophiles. The pH and the buffer salt concentration of the prelyo solution influenced the crystalline salt content in the final lyophile. The direction and magnitude of the pH shift in the frozen solution depended on both the initial pH and the buffer concentration. In light of the pH-sensitive nature of a significant fraction of pharmaceuticals (especially proteins), extreme care is needed in both the buffer selection and its concentration.« less

Thermodynamic effects of calcium and iron oxides on crystal phase formation in synthetic gasifier slags containing from 0 to 27wt.% V 2O 3

DOE PAGES

Nakano, Jinichiro; Duchesne, Marc; Bennett, James; ...

2014-11-15

Thermodynamic phase equilibria in synthetic slags (Al 2O 3–CaO–FeO–SiO 2–V 2O 3) were investigated with 0–27 wt.% vanadium oxide corresponding to industrial coal–petroleum coke (petcoke) feedstock blends in a simulated gasifier environment. Samples encompassing coal–petcoke mixed slag compositions were equilibrated at 1500 °C in a 64 vol.% CO/36 vol.% CO 2 atmosphere (Po 2 ≈ 10 –8 atm at 1500 °C) for 72 h, followed by rapid water quench, then analyzed by inductively coupled plasma optical emission spectrometry, X-ray diffractometry, and scanning electron microscopy with wavelength dispersive spectroscopy. With increasing CaO content, FeO content, or both; the slag homogeneity regionmore » expanded and a composition range exhibiting crystals was reduced. The mullite (Al 6Si 2O 13) crystalline phase was not present in the slags above 9 wt.% FeO while the karelianite (V 2O 3) crystalline phase was always present in compositions studied if a sufficient amount of vanadium existed in the slag. Furthermore, based on the present experimental equilibrium evaluation, a set of isothermal phase diagrams showing effects of CaO and FeO on thermodynamic phase stabilities in the vanadium-bearing slags is proposed. Some uses of the diagrams for potential industrial practice are discussed.« less

1D and 3D Polymeric Manganese(II) Thiolato Complexes: Synthesis, Structure, and Properties of    ∞3[Mn4(SPh)8] and ∞1[Mn(SMes)2].

PubMed

Eichhöfer, Andreas; Lebedkin, Sergei

2018-01-16

Reactions of [Mn{N(SiMe 3 ) 2 } 2 ] 2 with 2.1 equiv of RSH, R = Ph or Mes = C 6 H 2 -2,4,6-(CH 3 ) 3 , yield compounds of the formal composition "Mn(SR) 2 ". Single-crystal X-ray diffraction reveals that ∞ 1 [Mn(SMes) 2 ] forms one-dimensional chains in the crystal via μ 2 -SMes bridges, whereas ∞ 3 [Mn 4 (SPh) 8 ] comprises a three-dimensional network in which adamantanoid cages composed of four Mn atoms and six μ 2 -bridging SPh ligands are connected in three dimensions by doubly bridging SPh ligands. Thermogravimetric analysis and powder diffractometry indicate an reversible uptake of solvent molecules (tetrahydrofuran) into the channels of ∞ 1 [Mn(SMes) 2 ]. Magnetic measurements reveal antiferromagnetic coupling for both compounds with J = -8.2 cm -1 ( ∞ 1 [Mn(SMes) 2 ]) and -10.0 cm -1 ( ∞ 3 [Mn 4 (SPh) 8 ]), respectively. Their optical absorption and photoluminescence (PL) excitation spectra display characteristic d-d bands of Mn 2+ ions in the visible spectral region. Both compounds emit bright phosphorescence at ∼800 nm at low temperatures (<100 K). However, only ∞ 1 [Mn(SMes) 2 ] retains a moderately intense emission at ambient temperature (with a quantum yield of 1.2%). Similar PL properties are also found for the related selenolate complexes ∞ 1 [Mn(SeR) 2 ] (R = Ph, Mes).

Synthesis of ZnS films on Si(100) wafers by using chemical bath deposition assisted by the complexing agent ethylenediamine

NASA Astrophysics Data System (ADS)

Zhu, He-Jie; Wang, Xue-Mei; Gao, Xiao-Yong

2015-07-01

Low-cost synthesis of high-quality ZnS films on silicon wafers is of much importance to the ZnSbased heterojunction blue light-emitting device integrated with silicon. Thus, a series of ZnS films were chemically synthesized at low cost on Si(100) wafers at 353 K under a mixed acidic solution with a pH of 4 with zinc acetate and thioacetamide as precursors and with ethylenediamine and hydrochloric acid as the complexing agent and the pH value modifier, respectively. The effects of the ethylenediamine concentration on the crystallization, surface morphology, and optical properties of the ZnS films were investigated by using X-ray diffractometry, scanning electron microscopy, spectrophotometry, and fluorescence spectroscopy. A mechanism for the formation of ZnS film under an acidic condition was also proposed. All of the ZnS films were polycrystalline in nature, with a dominant cubic phase and a small amounts of hexagonal phases. The crystallization and the surface pattern of the films were clearly improved with increasing ethylenediamine concentration due to its enhanced complexing role. The absorption edge of the films almost underwent a blue shift with increasing ethylenediamine concentration, which was largely attributed to the quantum confinement effects caused by the small particle size of the polycrystalline ZnS films. Defect species and the corresponding strengths of the ZnS films were strongly affected by the ethylenediamine concentration.

A short working distance multiple crystal x-ray spectrometer

USGS Publications Warehouse

Dickinson, B.; Seidler, G.T.; Webb, Z.W.; Bradley, J.A.; Nagle, K.P.; Heald, S.M.; Gordon, R.A.; Chou, I.-Ming

2008-01-01

For x-ray spot sizes of a few tens of microns or smaller, a millimeter-sized flat analyzer crystal placed ???1 cm from the sample will exhibit high energy resolution while subtending a collection solid angle comparable to that of a typical spherically bent crystal analyzer (SBCA) at much larger working distances. Based on this observation and a nonfocusing geometry for the analyzer optic, we have constructed and tested a short working distance (SWD) multicrystal x-ray spectrometer. This prototype instrument has a maximum effective collection solid angle of 0.14 sr, comparable to that of 17 SBCA at 1 m working distance. We find good agreement with prior work for measurements of the Mn K?? x-ray emission and resonant inelastic x-ray scattering for MnO, and also for measurements of the x-ray absorption near-edge structure for Dy metal using L??2 partial-fluorescence yield detection. We discuss future applications at third- and fourth-generation light sources. For concentrated samples, the extremely large collection angle of SWD spectrometers will permit collection of high-resolution x-ray emission spectra with a single pulse of the Linac Coherent Light Source. The range of applications of SWD spectrometers and traditional multi-SBCA instruments has some overlap, but also is significantly complementary. ?? 2008 American Institute of Physics.

Production, purification, crystallization and preliminary X-ray analysis of adeno-associated virus serotype 8

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

Lane, Michael Douglas; Nam, Hyun-Joo; Padron, Eric

2005-06-01

The production, purification, crystallization and preliminary X-ray crystallographic analysis of adeno-associated virus serotype 8 is reported. Adeno-associated viruses (AAVs) are actively being developed for clinical gene-therapy applications and the efficiencies of the vectors could be significantly improved by a detailed understanding of their viral capsid structures and the structural determinants of their tissue-transduction interactions. AAV8 is ∼80% identical to the more widely studied AAV2, but its liver-transduction efficiency is significantly greater than that of AAV2 and other serotypes. The production, purification, crystallization and preliminary X-ray crystallographic analysis of AAV8 viral capsids are reported. The crystals diffract X-rays to 3.0 Åmore » resolution using synchrotron radiation and belong to the hexagonal space group P6{sub 3}22, with unit-cell parameters a = 257.5, c = 443.5 Å. The unit cell contains two viral particles, with ten capsid viral protein monomers per crystallographic asymmetric unit.« less

Cs2AgBiBr6 single-crystal X-ray detectors with a low detection limit

NASA Astrophysics Data System (ADS)

Pan, Weicheng; Wu, Haodi; Luo, Jiajun; Deng, Zhenzhou; Ge, Cong; Chen, Chao; Jiang, Xiaowei; Yin, Wan-Jian; Niu, Guangda; Zhu, Lujun; Yin, Lixiao; Zhou, Ying; Xie, Qingguo; Ke, Xiaoxing; Sui, Manling; Tang, Jiang

2017-11-01

Sensitive X-ray detection is crucial for medical diagnosis, industrial inspection and scientific research. The recently described hybrid lead halide perovskites have demonstrated low-cost fabrication and outstanding performance for direct X-ray detection, but they all contain toxic Pb in a soluble form. Here, we report sensitive X-ray detectors using solution-processed double perovskite Cs2AgBiBr6 single crystals. Through thermal annealing and surface treatment, we largely eliminate Ag+/Bi3+ disordering and improve the crystal resistivity, resulting in a detector with a minimum detectable dose rate as low as 59.7 nGyair s-1, comparable to the latest record of 0.036 μGyair s-1 using CH3NH3PbBr3 single crystals. Suppressed ion migration in Cs2AgBiBr6 permits relatively large external bias, guaranteeing efficient charge collection without a substantial increase in noise current and thus enabling the low detection limit.

Analysis and implementation of a space resolving spherical crystal spectrometer for x-ray Thomson scattering experiments.

PubMed

Harding, E C; Ao, T; Bailey, J E; Loisel, G; Sinars, D B; Geissel, M; Rochau, G A; Smith, I C

2015-04-01

The application of a space-resolving spectrometer to X-ray Thomson Scattering (XRTS) experiments has the potential to advance the study of warm dense matter. This has motivated the design of a spherical crystal spectrometer, which is a doubly focusing geometry with an overall high sensitivity and the capability of providing high-resolution, space-resolved spectra. A detailed analysis of the image fluence and crystal throughput in this geometry is carried out and analytical estimates of these quantities are presented. This analysis informed the design of a new spectrometer intended for future XRTS experiments on the Z-machine. The new spectrometer collects 6 keV x-rays with a spherically bent Ge (422) crystal and focuses the collected x-rays onto the Rowland circle. The spectrometer was built and then tested with a foam target. The resulting high-quality spectra prove that a spherical spectrometer is a viable diagnostic for XRTS experiments.

Crystallization and preliminary X-ray diffraction studies of θ-toxin (perfringolysin O), a pore-forming cytolysin of Clostridium perfringens

NASA Astrophysics Data System (ADS)

Sugahara, Mitsuaki; Sekino-Suzuki, Naoko; Ohno-Iwashita, Yoshiko; Miki, Kunio

1996-10-01

θ-Toxin (perfringolysin O), a cholesterol-binding, pore-forming cytolysin of Clostridium perfringens type A was crystallized by the vapor diffusion procedure using polyethyleneglycol 4000 and sodium chloride as precipitants in 2-(cyclohexylamino)ethanesulfonic acid (CHES) buffer at pH 9.5. The diffraction patterns of precession photographs indicated that the crystals belong to the orthorhombic system and the space group C222 1 with unit-cell dimensions of a = 47.7 Å, b = 182.0 Å and c = 175.8 Å. Assuming that the asymmetric unit contains one or two molecules (Mw 52 700), the Vm value is calculated as 3.6 or 1.8 Å 3/dalton, respectively. The crystals diffract X-rays to at least 3 Å resolution and are suitable for high resolution X-ray crystal structure determination.

Crystallization and preliminary X-ray diffraction study of recombinant ribokinase from Thermus Species 2.9

NASA Astrophysics Data System (ADS)

Abramchik, Yu. A.; Timofeev, V. I.; Muravieva, T. I.; Esipov, R. S.; Kuranova, I. P.

2016-11-01

Ribokinase from a thermophilic strain of Thermus species 2.9 belonging to the carbohydrate ribokinase family (EC 2.7.1.15) was isolated, purified, and crystallized. The crystallization conditions were found by the vapor-diffusion technique and were then optimized to apply the capillary counter-diffusion technique. The X-ray diffraction data set was collected from the crystals, which were grown by the counter-diffusion technique, at the SPring-8 synchrotron radiation facility to 2.87 Å resolution. The crystals belong to sp. gr. P1211 and have the following unit-cell parameters: a = 81.613 Å, b = 156.132 Å, c = 87.714 Å, α = γ = 90°, β = 103.819°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the protein by the molecular-replacement method.

Synthesis, crystal structure, vibrational spectroscopy and photoluminescence of new hybrid compound containing chlorate anions of stanate (II)

NASA Astrophysics Data System (ADS)

Lassoued, Mohamed Saber; Abdelbaky, Mohammed S. M.; Lassoued, Abdelmajid; Meroño, Rafael Mendoza; Gadri, Abdellatif; Ammar, Salah; Ben Salah, Abdelhamid; García-Granda, Santiago

2017-08-01

The present work aimed at studying a new organic-inorganic bis (4-amino quinolinium) hexachloro stanate (II) dihydrate compound. It was prepared and characterized by single crystal X-ray diffraction, X-ray powder, Hirshfeld surface, Spectroscopy measurement, thermal study and photoluminescence properties. It was found to crystallize in the monoclinic system (P21/c space group) with the following lattice parameters: a = 7.2558(6) Å, b = 13.4876(5) Å, c = 17.2107(13) Å, β = 102.028 (12)°. Its crystal structure was determined and refined down to an R value of 0.06 and a wR value of 0.087. The structure consisted of two different alternating organic-inorganic layers. The crystal packing was stabilized by Nsbnd H⋯Cl and Osbnd H⋯Cl hydrogen bonds and π-π interactions. Hirshfeld surface analysis was used to investigate intermolecular interactions, as well 2D finger plots were conducted to reveal the contribution of these interactions in the crystal structure quantitatively. The X-ray powder is in agreement with the X-ray structure. Scanning electronic microscopy (SEM) was carried out. Furthermore, the room temperature Infra Red (IR) spectrum of the title compound was analyzed on the basis of data found in the literature. Solid state 13C NMR spectrum shows ten signals, confirming the solid state structure determined by X-ray diffraction. Thermal analysis shows two anomalies at 380 and 610 °C. The optical properties of the crystal were studied using optical absorption UV-visible and photoluminescence (PL) spectroscopy, which were investigated at room temperature.

Feasibility Studies of Parametric X-rays Use in a Medical Environment

NASA Astrophysics Data System (ADS)

Sones, Bryndol; Danon, Yaron; Blain, Ezekiel

2009-03-01

Parametric X-rays (PXR) are produced from the interaction of relativistic electrons with the periodic structure of crystal materials. Smooth X-ray energy tunability is achieved by rotating the crystal with respects to the electron beam direction. Experiments at the Rensselaer Polytechnic Institute 60-MeV LINAC produce quasi-monochromatic X-rays (6-35 keV) from various target crystals to include highly oriented pyrolytic graphite (HOPG), LiF, Si, Ge, Cu, and W using electron beam currents up to 6 uA. These experiments demonstrate the first PXR images and some of the merits of thin metallic crystals. Recent experiments with a 100-μm thick Cu crystal improve the Cu PXR (with energy ˜12 keV) to Cu fluorescence ratio by a factor of 20 compared to a 1 mm-thick Cu crystal. This study uses Monte Carlo techniques to investigate (1) PXR dose compared to emissions from simulated Mo, Rh, and W anodes for mammography applications and (2) electron scattering effects when considering LiF111, Si111, and Cu111 PXR production using electron beams with energies of 20-30 MeV. Advantages in using monochromatic PXR compared to X-rays from Mo and Rh anodes in mammography applications result in a dose per incident photon reduction by a factor of 2. Using 20 MeV electrons, the thinner Cu111 crystal for 15 keV PXR production results in an electron scattering angle of 30.7+/-0.2 mrad offering the best potential for PXR from lower energy electrons.

In Situ X-Ray Studies of Crystallization Kinetics and Ordering in Functional Organic and Hybrid Materials

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

Yang, Bin; Keum, Jong K.; Geohegan, David B.

In-Situ and time-resolved X-ray scattering and diffraction is dedicated to yielding the change of structural information as the materials are processed or grown in a controlled environment. In this chapter, we introduce the use of in situ and time-resolved X-ray techniques to understand molecular packing, crystal orientation, and phase transformation during the synthesis and processing of functional organic semiconductors, organic nanowires, and hybrid perovskite materials.

Acoustically Mounted Microcrystals Yield High Resolution X-ray Structures†,‡

PubMed Central

Soares, Alexei S.; Engel, Matthew A.; Stearns, Richard; Datwani, Sammy; Olechno, Joe; Ellson, Richard; Skinner, John M.; Allaire, Marc; Orville, Allen M.

2011-01-01

We demonstrate a general strategy to determine structures from showers of microcrystals. It uses acoustic droplet ejection (ADE) to transfer 2.5 nanoliter droplets from the surface of microcrystal slurries, through the air, and onto mounting micromesh pins. Individual microcrystals are located by raster-scanning a several micron X-ray beam across the cryocooled micromeshes. X-ray diffraction datasets merged from several micron-sized crystals are used to solve 1.8 Å resolution crystal structures. PMID:21542590

Impact of intense x-ray pulses on a NaI(Tl)-based gamma camera

NASA Astrophysics Data System (ADS)

Koppert, W. J. C.; van der Velden, S.; Steenbergen, J. H. L.; de Jong, H. W. A. M.

2018-03-01

In SPECT/CT systems x-ray and γ-ray imaging is performed sequentially. Simultaneous acquisition may have advantages, for instance in interventional settings. However, this may expose a gamma camera to relatively high x-ray doses and deteriorate its functioning. We studied the NaI(Tl) response to x-ray pulses with a photodiode, PMT and gamma camera, respectively. First, we exposed a NaI(Tl)-photodiode assembly to x-ray pulses to investigate potential crystal afterglow. Next, we exposed a NaI(Tl)-PMT assembly to 10 ms LED pulses (mimicking x-ray pulses) and measured the response to flashing LED probe-pulses (mimicking γ-pulses). We then exposed the assembly to x-ray pulses, with detector entrance doses of up to 9 nGy/pulse, and analysed the response for γ-pulse variations. Finally, we studied the response of a Siemens Diacam gamma camera to γ-rays while exposed to x-ray pulses. X-ray exposure of the crystal, read out with a photodiode, revealed 15% afterglow fraction after 3 ms. The NaI(Tl)-PMT assembly showed disturbances up to 10 ms after 10 ms LED exposure. After x-ray exposure however, responses showed elevated baselines, with 60 ms decay-time. Both for x-ray and LED exposure and after baseline subtraction, probe-pulse analysis revealed disturbed pulse height measurements shortly after exposure. X-ray exposure of the Diacam corroborated the elementary experiments. Up to 50 ms after an x-ray pulse, no events are registered, followed by apparent energy elevations up to 100 ms after exposure. Limiting the dose to 0.02 nGy/pulse prevents detrimental effects. Conventional gamma cameras exhibit substantial dead-time and mis-registration of photon energies up to 100 ms after intense x-ray pulses. This is due PMT limitations and due to afterglow in the crystal. Using PMTs with modified circuitry, we show that deteriorative afterglow effects can be reduced without noticeable effects on the PMT performance, up to x-ray pulse doses of 1 nGy.

A simultaneous multiple angle-wavelength dispersive X-ray reflectometer using a bent-twisted polychromator crystal

PubMed Central

Matsushita, Tadashi; Arakawa, Etsuo; Voegeli, Wolfgang; Yano, Yohko F.

2013-01-01

An X-ray reflectometer has been developed, which can simultaneously measure the whole specular X-ray reflectivity curve with no need for rotation of the sample, detector or monochromator crystal during the measurement. A bent-twisted crystal polychromator is used to realise a convergent X-ray beam which has continuously varying energy E (wavelength λ) and glancing angle α to the sample surface as a function of horizontal direction. This convergent beam is reflected in the vertical direction by the sample placed horizontally at the focus and then diverges horizontally and vertically. The normalized intensity distribution of the reflected beam measured downstream of the specimen with a two-dimensional pixel array detector (PILATUS 100K) represents the reflectivity curve. Specular X-ray reflectivity curves were measured from a commercially available silicon (100) wafer, a thin gold film coated on a silicon single-crystal substrate and the surface of liquid ethylene glycol with data collection times of 0.01 to 1000 s using synchrotron radiation from a bending-magnet source of a 6.5 GeV electron storage ring. A typical value of the simultaneously covered range of the momentum transfer was 0.01–0.45 Å−1 for the silicon wafer sample. The potential of this reflectometer for time-resolved X-ray studies of irreversible structural changes is discussed. PMID:23254659

An x-ray diffraction study of microstructural deformation induced by cyclic loading of selected steels

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

Fourspring, P.M.; Pangborn, R.N.

1996-06-01

X-ray double crystal diffractometry (XRDCD) was used to assess cyclic microstructural deformation in a face centered cubic (fcc) steel (AISI304) and a body centered cubic (bcc) steel (SA508 class 2). The first objective of the investigation was to determine if XRDCD could be used to effectively monitor cyclic microstructural deformation in polycrystalline Fe alloys. A second objective was to study the microstructural deformation induced by cyclic loading of polycrystalline Fe alloys. The approach used in the investigation was to induce fatigue damage in a material and to characterize the resulting microstructural deformation at discrete fractions of the fatigue life ofmore » the material. Also, characterization of microstructural deformation was carried out to identify differences in the accumulation of damage from the surface to the bulk, focusing on the following three regions: near surface (0--10 {micro}m), subsurface (10--300 {micro}m), and bulk. Characterization of the subsurface region was performed only on the AISI304 material because of the limited availability of the SA508 material. The results from the XRDCD data indicate a measurable change induced by fatigue from the initial state to subsequent states of both the AISI304 and the SA508 materials. Therefore, the XRDCD technique was shown to be sensitive to the microstructural deformation caused by fatigue in steels; thus, the technique can be used to monitor fatigue damage in steels. In addition, for the AISI304 material, the level of cyclic microstructural deformation in the bulk material was found to be greater than the level in the near surface material. In contrast, previous investigations have shown that the deformation is greater in the near surface than the bulk for Al alloys and bcc Fe alloys.« less

Electronic, optical and photocatalytic behavior of Mn, N doped and co-doped TiO{sub 2}: Experiment and simulation

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

Zhao, Ya Fei; Li, Can, E-mail: canli1983@gmail.com; Lu, Song

2016-03-15

The crystal phase structure, surface morphology, chemical states and optical properties of Mn, N mono-doped and co-doped TiO{sub 2} nanoparticles were investigated by X-ray powder diffractometry, Raman spectra, scanning electron microscopy, X-ray photoelectron spectroscopy and UV–vis diffuse reflectance spectroscopy. Meanwhile, geometry structures, formation energies, electronic and optical properties of all systems have been also analyzed by density functional theory. The results showed that the band gap values and the carrier mobility in the valence band, conduction band and impurity levels have a synergetic influence on the visible-light absorption and photocatalytic activity of the doped TiO{sub 2}. The number and themore » carrier mobility of impurity level jointly influence the photocatalytic activity of catalyst under visible-light. Especially, the photocatalytic activity of Mn-2N co-doped TiO{sub 2} beyond three-fold than that of pure TiO{sub 2} under visible-light. - Graphical abstract: The ILs formed by N-2p orbital in N single doped specimen lie above the VB, while the ILs formed by Mn-3d orbital in Mn single doped specimen appear below the CB. However, a large amount of ILs formed by N-2p orbital and Mn-3d orbital in N and Mn codoped specimens. The band gap values and the carrier mobility in the valence band, conduction band and impurity levels have a synergetic influence on the visible-light absorption and photocatalytic activity of the doped TiO{sub 2}. The number and the carrier mobility of impurity level jointly influence the photocatalytic activity of catalyst under visible-light.« less

Blue–green afterglow of BaAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors

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

Zhai, Bao-gai; Ma, Qing-lan; School of Electronics and Information, Nantong University, Jiangsu 226019

Highlights: • Afterglow can be achieved when Eu{sup 2+} is absent in the DyAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors. • The afterglow of DyAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors is discernible to naked eyes for minutes. • Dy{sup 3+} introduced trap centers are believed to be responsible for the afterglow. - Abstract: Dy{sup 3+} doped barium aluminate (BaAl{sub 2}O{sub 4}:Dy{sup 3+}) phosphors were prepared via the sol–gel combustion route at the ignition temperature of 600 °C. The phosphors were characterized with X-ray diffractometry, scanning electron microscopy, transmission electron microscopy, photoluminescence spectroscopy, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. Regardless of themore » absence of Eu{sup 2+} luminescent centers, broadband blue–green afterglow with its peak at about 490 nm was recorded in the BaAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors. The decay profile of the blue–green afterglow can be best fitted into a two-component exponential function with the two lifetime decay constants to be 8.81 and 45.25 s, respectively. The observation of blue–green afterglow from BaAl{sub 2}O{sub 4}:Dy{sup 3+} in the absence of Eu{sup 2+} provides unique opportunity in unveiling the afterglow mechanisms of rare-earth doped alkaline-metal aluminates. Possible mechanisms on the blue–green afterglow in BaAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors are discussed in terms of the Dy{sup 3+} ions introduced trap centers as well as luminescent centers in the crystal lattice.« less

Density functional study for the bridged dinuclear center based on a high-resolution X-ray crystal structure of ba3 cytochrome c oxidase from Thermus thermophilus.

PubMed

Du, Wen-Ge Han; Noodleman, Louis

2013-12-16

Strong electron density for a peroxide type dioxygen species bridging the Fea3 and CuB dinuclear center (DNC) was observed in the high-resolution (1.8 Å) X-ray crystal structures (PDB entries 3S8G and 3S8F) of ba3 cytochrome c oxidase (CcO) from Thermus thermophilus. The crystals represent the as-isolated X-ray photoreduced CcO structures. The bridging peroxide was proposed to arise from the recombination of two radiation-produced HO(•) radicals formed either very near to or even in the space between the two metals of the DNC. It is unclear whether this peroxide species is in the O2(2-), O2(•)(-), HO2(-), or the H2O2 form and what is the detailed electronic structure and binding geometry including the DNC. In order to answer what form of this dioxygen species was observed in the DNC of the 1.8 Å X-ray CcO crystal structure (3S8G), we have applied broken-symmetry density functional theory (BS-DFT) geometric and energetic calculations (using OLYP potential) on large DNC cluster models with different Fea3-CuB oxidation and spin states and with O2(2-), O2(•)(-), HO2(-), or H2O2 in the bridging position. By comparing the DFT optimized geometries with the X-ray crystal structure (3S8G), we propose that the bridging peroxide is HO2(-). The X-ray crystal structure is likely to represent the superposition of the Fea3(2+)-(HO2(-))-CuB(+) DNC's in different states (Fe(2+) in low spin (LS), intermediate spin (IS), or high spin (HS)) with the majority species having the proton of the HO2(-) residing on the oxygen atom (O1) which is closer to the Fea3(2+) site in the Fea3(2+)-(HO-O)(-)-CuB(+) conformation. Our calculations show that the side chain of Tyr237 is likely trapped in the deprotonated Tyr237(-) anion form in the 3S8G X-ray crystal structure.

Site partitioning of Cr3+ in the trichroic alexandrite BeAl2O4:Cr3+ crystal: contribution from x-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Bordage, Amélie; Rossano, Stéphanie; Horn, Adolf Heinrich; Fuchs, Yves

2012-06-01

X-ray absorption spectroscopy measurements at the Cr K-edge of a trichroic crystal of alexandrite BeAl2O4:Cr3+ for different orientations of the crystal with respect to the polarization and direction of the x-ray incident beam have been performed. Analysis of the experimental spectra with the help of first-principles calculations of x-ray absorption spectra allowed us to estimate the proportion of chromium Cr3+ cations among the two different octahedral sites of the alexandrite structure (70% in the Cs site-30% in the Ci site). The methodology presented in this work opens up new possibilities in the field of mineralogy for the study of complex minerals containing several sites potentially occupied by several transition elements or for solid solutions.

Quantitative analysis of crystalline pharmaceuticals in tablets by pattern-fitting procedure using X-ray diffraction pattern.

PubMed

Takehira, Rieko; Momose, Yasunori; Yamamura, Shigeo

2010-10-15

A pattern-fitting procedure using an X-ray diffraction pattern was applied to the quantitative analysis of binary system of crystalline pharmaceuticals in tablets. Orthorhombic crystals of isoniazid (INH) and mannitol (MAN) were used for the analysis. Tablets were prepared under various compression pressures using a direct compression method with various compositions of INH and MAN. Assuming that X-ray diffraction pattern of INH-MAN system consists of diffraction intensities from respective crystals, observed diffraction intensities were fitted to analytic expression based on X-ray diffraction theory and separated into two intensities from INH and MAN crystals by a nonlinear least-squares procedure. After separation, the contents of INH were determined by using the optimized normalization constants for INH and MAN. The correction parameter including all the factors that are beyond experimental control was required for quantitative analysis without calibration curve. The pattern-fitting procedure made it possible to determine crystalline phases in the range of 10-90% (w/w) of the INH contents. Further, certain characteristics of the crystals in the tablets, such as the preferred orientation, size of crystallite, and lattice disorder were determined simultaneously. This method can be adopted to analyze compounds whose crystal structures are known. It is a potentially powerful tool for the quantitative phase analysis and characterization of crystals in tablets and powders using X-ray diffraction patterns. Copyright 2010 Elsevier B.V. All rights reserved.

Crystallization and preliminary X-ray diffraction analysis of recombinant phosphoribosylpyrophosphate synthetase from the Thermophilic thermus thermophilus strain HB27

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

Abramchik, Yu. A.; Timofeev, V. I., E-mail: tostars@mail.ru; Muravieva, T. I.

2017-01-15

Phosphoribosylpyrophosphate synthetases (PRPP synthetases) are among the key enzymes essential for vital functions of organisms and are involved in the biosynthesis of purine and pyrimidine nucleotides, coenzymes, and the amino acids histidine and tryptophan. These enzymes are used in biotechnology for the combined chemoenzymatic synthesis of natural nucleotide analogs. Recombinant phosphoribosylpyrophosphate synthetase I from the thermophilic strain HB27 of the bacterium Thermus thermophilus (T. th HB27) has high thermal stability and shows maximum activity at 75°Ð¡, due to which this enzyme holds promise for biotechnological applications. In order to grow crystals and study them by X-ray crystallography, an enzyme sample,more » which was produced using a highly efficient producer strain, was purified by affinity and gel-filtration chromatography. The screening of crystallization conditions was performed by the vapor-diffusion technique. The crystals of the enzyme suitable for X-ray diffraction were grown by the counter-diffusion method through a gel layer. These crystals were used to collect the X-ray diffraction data set at the SPring-8 synchrotron radiation facility (Japan) to 3-Å resolution. The crystals belong to sp. gr. P2{sub 1} and have the following unitcell parameters: a = 107.7 Å, b = 112.6 Å, c = 110.2 Å, α = γ = 90°, β = 116.6°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the enzyme at 3.0-Å resolution.« less

Crystallization and preliminary X-ray diffraction analysis of recombinant phosphoribosylpyrophosphate synthetase from the Thermophilic thermus thermophilus strain HB27

NASA Astrophysics Data System (ADS)

Abramchik, Yu. A.; Timofeev, V. I.; Muravieva, T. I.; Sinitsyna, E. V.; Esipov, R. S.; Kuranova, I. P.

2017-01-01

Phosphoribosylpyrophosphate synthetases (PRPP synthetases) are among the key enzymes essential for vital functions of organisms and are involved in the biosynthesis of purine and pyrimidine nucleotides, coenzymes, and the amino acids histidine and tryptophan. These enzymes are used in biotechnology for the combined chemoenzymatic synthesis of natural nucleotide analogs. Recombinant phosphoribosylpyrophosphate synthetase I from the thermophilic strain HB27 of the bacterium Thermus thermophilus ( T. th HB27) has high thermal stability and shows maximum activity at 75°C, due to which this enzyme holds promise for biotechnological applications. In order to grow crystals and study them by X-ray crystallography, an enzyme sample, which was produced using a highly efficient producer strain, was purified by affinity and gel-filtration chromatography. The screening of crystallization conditions was performed by the vapor-diffusion technique. The crystals of the enzyme suitable for X-ray diffraction were grown by the counter-diffusion method through a gel layer. These crystals were used to collect the X-ray diffraction data set at the SPring-8 synchrotron radiation facility (Japan) to 3-Å resolution. The crystals belong to sp. gr. P21 and have the following unitcell parameters: a = 107.7 Å, b = 112.6 Å, c = 110.2 Å, α = γ = 90°, β = 116.6°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the enzyme at 3.0-Å resolution.

Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

NASA Technical Reports Server (NTRS)

Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

2010-01-01

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

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

Ovchinnikova, E. N.; Rogalev, A.; Wilhelm, F.

The local electronic structure of copper ions in a copper metaborate CuB{sub 2}O{sub 4} crystal is studied on the ESRF synchrotron using X-ray absorption polarization-dependent spectroscopy. The X-ray natural circular dichroism near the K absorption edge of copper is measured in the direction that is perpendicular to crystal axis c. The data obtained indicate the presence of hybridized p–d electronic states of copper. Theoretical calculations are used to separate the contributions of the two crystallographically nonequivalent positions of copper atoms in the unit cell of CuB{sub 2}O{sub 4} to the absorption and X-ray circular dichroism spectra of the crystal.

Crystallization and preliminary X-ray crystallographic analysis of carboxyl-terminal region 4 of SigR from Streptomyces coelicolor A3(2)

PubMed Central

Kim, Keon Young; Kim, Sunmin; Park, Jeong Kuk; Song, HyoJin; Park, SangYoun

2014-01-01

Full-length SigR from Streptomyces coelicolor A3(2) was overexpressed in Escherichia coli, purified and submitted to crystallization trials using either polyethylene glycol 3350 or 4000 as a precipitant. X-ray diffraction data were collected to 2.60 Å resolution under cryoconditions using synchrotron X-rays. The crystal packs in space group P43212, with unit-cell parameters a = b = 42.14, c = 102.02 Å. According to the Matthews coefficient, the crystal asymmetric unit cannot contain the full-length protein. Molecular replacement with the known structures of region 2 and region 4 as independent search models indicates that the crystal contains only the −35 element-binding carboxyl-terminal region 4 of full-length SigR. Mass-spectrometric analysis of the harvested crystal confirms this, suggesting a crystal volume per protein weight (V M) of 2.24 Å3 Da−1 and 45.1% solvent content. PMID:24915084

NARROW LINE ABSORPTION IN CACO3.

DTIC Science & Technology

CARBONATES), (*CALCIUM COMPOUNDS, (*ABSORPTION SPECTRA, CALCITE), (*CALCITE, RADIATION EFFECTS), ELECTRON PARAMAGNETIC RESONANCE, SINGLE CRYSTALS , NEUTRONS, X RAYS, GAMMA RAYS, IONS, CRYSTAL DEFECTS, PARAMAGNETIC RESONANCE.

Novel ultra-lightweight and high-resolution MEMS x-ray optics

NASA Astrophysics Data System (ADS)

Mitsuishi, Ikuyuki; Ezoe, Yuichiro; Takagi, Utako; Mita, Makoto; Riveros, Raul; Yamaguchi, Hitomi; Kato, Fumiki; Sugiyama, Susumu; Fujiwara, Kouzou; Morishita, Kohei; Nakajima, Kazuo; Fujihira, Shinya; Kanamori, Yoshiaki; Yamasaki, Noriko Y.; Mitsuda, Kazuhisa; Maeda, Ryutaro

2009-05-01

We have been developing ultra light-weight X-ray optics using MEMS (Micro Electro Mechanical Systems) technologies.We utilized crystal planes after anisotropic wet etching of silicon (110) wafers as X-ray mirrors and succeeded in X-ray reflection and imaging. Since we can etch tiny pores in thin wafers, this type of optics can be the lightest X-ray telescope. However, because the crystal planes are alinged in certain directions, we must approximate ideal optical surfaces with flat planes, which limits angular resolution of the optics on the order of arcmin. In order to overcome this issue, we propose novel X-ray optics based on a combination of five recently developed MEMS technologies, namely silicon dry etching, X-ray LIGA, silicon hydrogen anneal, magnetic fluid assisted polishing and hot plastic deformation of silicon. In this paper, we describe this new method and report on our development of X-ray mirrors fabricated by these technologies and X-ray reflection experiments of two types of MEMS X-ray mirrors made of silicon and nickel. For the first time, X-ray reflections on these mirrors were detected in the angular response measurements. Compared to model calculations, surface roughness of the silicon and nickel mirrors were estimated to be 5 nm and 3 nm, respectively.

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt

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

Soares, Alexei S.; Mullen, Jeffrey D.; Parekh, Ruchi M.

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltdin situmicro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ~100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face thatmore » preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. Lastly, high-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies.« less

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt.

PubMed

Soares, Alexei S; Mullen, Jeffrey D; Parekh, Ruchi M; McCarthy, Grace S; Roessler, Christian G; Jackimowicz, Rick; Skinner, John M; Orville, Allen M; Allaire, Marc; Sweet, Robert M

2014-11-01

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltd in situ micro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ∼100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face that preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. High-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies.

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt

DOE PAGES

Soares, Alexei S.; Mullen, Jeffrey D.; Parekh, Ruchi M.; ...

2014-10-09

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltdin situmicro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ~100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face thatmore » preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. Lastly, high-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies.« less

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt

PubMed Central

Soares, Alexei S.; Mullen, Jeffrey D.; Parekh, Ruchi M.; McCarthy, Grace S.; Roessler, Christian G.; Jackimowicz, Rick; Skinner, John M.; Orville, Allen M.; Allaire, Marc; Sweet, Robert M.

2014-01-01

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltd in situ micro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ∼100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face that preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. High-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies. PMID:25343789

Femtosecond X-ray protein nanocrystallography

PubMed Central

Chapman, Henry N.; Fromme, Petra; Barty, Anton; White, Thomas A.; Kirian, Richard A.; Aquila, Andrew; Hunter, Mark S.; Schulz, Joachim; DePonte, Daniel P.; Weierstall, Uwe; Doak, R. Bruce; Maia, Filipe R. N. C.; Martin, Andrew V.; Schlichting, Ilme; Lomb, Lukas; Coppola, Nicola; Shoeman, Robert L.; Epp, Sascha W.; Hartmann, Robert; Rolles, Daniel; Rudenko, Artem; Foucar, Lutz; Kimmel, Nils; Weidenspointner, Georg; Holl, Peter; Liang, Mengning; Barthelmess, Miriam; Caleman, Carl; Boutet, Sébastien; Bogan, Michael J.; Krzywinski, Jacek; Bostedt, Christoph; Bajt, Saša; Gumprecht, Lars; Rudek, Benedikt; Erk, Benjamin; Schmidt, Carlo; Hömke, André; Reich, Christian; Pietschner, Daniel; Strüder, Lothar; Hauser, Günter; Gorke, Hubert; Ullrich, Joachim; Herrmann, Sven; Schaller, Gerhard; Schopper, Florian; Soltau, Heike; Kühnel, Kai-Uwe; Messerschmidt, Marc; Bozek, John D.; Hau-Riege, Stefan P.; Frank, Matthias; Hampton, Christina Y.; Sierra, Raymond G.; Starodub, Dmitri; Williams, Garth J.; Hajdu, Janos; Timneanu, Nicusor; Seibert, M. Marvin; Andreasson, Jakob; Rocker, Andrea; Jönsson, Olof; Svenda, Martin; Stern, Stephan; Nass, Karol; Andritschke, Robert; Schröter, Claus-Dieter; Krasniqi, Faton; Bott, Mario; Schmidt, Kevin E.; Wang, Xiaoyu; Grotjohann, Ingo; Holton, James M.; Barends, Thomas R. M.; Neutze, Richard; Marchesini, Stefano; Fromme, Raimund; Schorb, Sebastian; Rupp, Daniela; Adolph, Marcus; Gorkhover, Tais; Andersson, Inger; Hirsemann, Helmut; Potdevin, Guillaume; Graafsma, Heinz; Nilsson, Björn; Spence, John C. H.

2012-01-01

X-ray crystallography provides the vast majority of macromolecular structures, but the success of the method relies on growing crystals of sufficient size. In conventional measurements, the necessary increase in X-ray dose to record data from crystals that are too small leads to extensive damage before a diffraction signal can be recorded1-3. It is particularly challenging to obtain large, well-diffracting crystals of membrane proteins, for which fewer than 300 unique structures have been determined despite their importance in all living cells. Here we present a method for structure determination where single-crystal X-ray diffraction ‘snapshots’ are collected from a fully hydrated stream of nanocrystals using femtosecond pulses from a hard-X-ray free-electron laser, the Linac Coherent Light Source4. We prove this concept with nanocrystals of photosystem I, one of the largest membrane protein complexes5. More than 3,000,000 diffraction patterns were collected in this study, and a three-dimensional data set was assembled from individual photosystem I nanocrystals (~200 nm to 2 μm in size). We mitigate the problem of radiation damage in crystallography by using pulses briefer than the timescale of most damage processes6. This offers a new approach to structure determination of macromolecules that do not yield crystals of sufficient size for studies using conventional radiation sources or are particularly sensitive to radiation damage. PMID:21293373

The Formation Mechanism and Corrosion Resistance of a Composite Phosphate Conversion Film on AM60 Alloy.

PubMed

Chen, Jun; Lan, Xiangna; Wang, Chao; Zhang, Qinyong

2018-03-08

Magnesium alloy AM60 has high duc and toughness, which is expected to increase in demand for automotive applications. However, it is too active, and coatings have been extensively studied to prevent corrosion. In this work, a Ba-containing composite phosphate film has been prepared on the surface of AM60. The composition and formation mechanism of the film have been investigated using a scanning electronic microscope equipped with energy dispersive X-ray spectroscopy, Fourier transform infrared, X-ray photoelectron spectroscopy, and X-ray diffractometry tests. The corrosion resistance of the film has been measured by electrochemical and immersion tests. The results show that the deposition film has fully covered the substrate but there are some micro-cracks. The structure of the film is complex, and consists of MgHPO₄·3H₂O, MnHPO₄·2.25H₂O, BaHPO₄·3H₂O, BaMg₂(PO₄)₂, Mg₃(PO₄)₂·22H₂O, Ca₃(PO₄)₂·xH₂O, and some amorphous phases. The composite phosphate film has better anticorrosion performance than the AM60 and can protect the bare alloy from corrosion for more than 12 h in 0.6 M NaCl.

Influence of atmospheric pressure low-temperature plasma treatment on the shear bond strength between zirconia and resin cement.

PubMed

Ito, Yuki; Okawa, Takahisa; Fukumoto, Takahiro; Tsurumi, Akiko; Tatsuta, Mitsuhiro; Fujii, Takamasa; Tanaka, Junko; Tanaka, Masahiro

2016-10-01

Zirconia exhibits excellent strength and high biocompatibility in technological applications and it is has therefore been investigated for clinical applications and research. Before setting prostheses, a crown prosthesis inner surface is sandblasted with alumina to remove contaminants and form small cavities. This alumina sandblasting causes stress-induced phase transition of zirconia. Atmospheric-pressure low-temperature plasma has been applied in the dental industry, particularly for adhesives, as a surface treatment to activate the surface energy and remove contaminants. The purpose of this study was to examine the influence of atmospheric-pressure low-temperature plasma treatment on the shear bond strength between zirconia and adhesive resin cement. The surface treatment method was classified into three groups: untreated (Cont group), alumina sandblast treatment (Sb group), and atmospheric-pressure low-temperature plasma treatment (Ps group). Adhesive resin cement was applied to stainless steel and bonded to zirconia. Shear adhesion tests were performed after complete hardening of the cement. Multiple comparisons were performed using a one-way analysis of variance and the Bonferroni method. X-ray diffractometry was used to examine the change in zirconia crystal structure. Statistically significant differences were noted between the control and Sb groups and between the control and Ps groups. In contrast, no statistically significant differences were noted for the Ps and Sb bond strength. Atmospheric-pressure low-temperature plasma treatment did not affect the zirconia crystal structure. Atmospheric-pressure low-temperature plasma treatment improves the bonding strength of adhesive resin cement as effectively as alumina sandblasting, and does not alter the zirconia crystal structure. Copyright © 2016 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

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

DOE PAGES

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

2016-08-01

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

Oxidation and crystal field effects in uranium

NASA Astrophysics Data System (ADS)

Tobin, J. G.; Yu, S.-W.; Booth, C. H.; Tyliszczak, T.; Shuh, D. K.; van der Laan, G.; Sokaras, D.; Nordlund, D.; Weng, T.-C.; Bagus, P. S.

2015-07-01

An extensive investigation of oxidation in uranium has been pursued. This includes the utilization of soft x-ray absorption spectroscopy, hard x-ray absorption near-edge structure, resonant (hard) x-ray emission spectroscopy, cluster calculations, and a branching ratio analysis founded on atomic theory. The samples utilized were uranium dioxide (U O2) , uranium trioxide (U O3) , and uranium tetrafluoride (U F4) . A discussion of the role of nonspherical perturbations, i.e., crystal or ligand field effects, will be presented.

Growth and characterization of organic NLO material: Clobetasol propionate

NASA Astrophysics Data System (ADS)

Purusothaman, R.; Rajesh, P.; Ramasamy, P.

2015-06-01

Single crystals of clobetasol propionate (CP) have been grown by slow evaporation solution technique using mixed solvent of methanol-acetone. The grown crystals were subjected to single crystal X-ray diffraction analysis to confirm their lattice parameter and space group. The powder X-ray diffraction pattern of the grown CP has been indexed. Thermal analysis was performed to study the thermal stability of the grown crystals. Photoluminescence spectrum shows broad emission peak observed at 421 nm. Nonlinear optical studies were carried out for the grown crystal and second harmonic generation (SHG) efficiency was found in the crystal.

Calibration of a High Resolution X-ray Spectrometer for High-Energy-Density Plasmas on NIF

NASA Astrophysics Data System (ADS)

Kraus, B.; Gao, L.; Hill, K. W.; Bitter, M.; Efthimion, P.; Schneider, M. B.; Chen, H.; Ayers, J.; Beiersdorfer, P.; Liedahl, D.; Macphee, A. G.; Thorn, D. B.; Bettencourt, R.; Kauffman, R.; Le, H.; Nelson, D.

2017-10-01

A high-resolution, DIM-based (Diagnostic Instrument Manipulator) x-ray crystal spectrometer has been calibrated for and deployed at the National Ignition Facility (NIF) to diagnose plasma conditions and mix in ignition capsules near stagnation times. Two conical crystals in the Hall geometry focus rays from the Kr He- α, Ly- α, and He- β complexes onto a streak camera for time-resolved spectra, in order to measure electron density and temperature by observing Stark broadening and relative intensities of dielectronic satellites. Signals from these two crystals are correlated with a third crystal that time-integrates the intervening energy range. The spectrometer has been absolutely calibrated using a microfocus x-ray source, an array of CCD and single-photon-counting detectors, and K- and L-absorption edge filters. Measurements of the integrated reflectivity, energy range, and energy resolution for each crystal will be presented. The implications of the calibration on signal levels from NIF implosions and x-ray filter choices will be discussed. This work was performed under the auspices of the U.S. DoE by Princeton Plasma Physics Laboratory under contract DE-AC02-09CH11466 and by Lawrence Livermore National Laboratory under contract DE-AC52-07NA27344.

Nonlinear refraction properties of nickel oxide thin films at 800 nm

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

Melo, Ronaldo P. Jr. de; Silva, Blenio J. P. da; Santos, Francisco Eroni P. dos

2009-11-01

Measurements of the nonlinear refractive index, n{sub 2}, of nickel oxide films prepared by controlled oxidation of nickel films deposited on substrates of soda-lime glass are reported. The structure and morphology of the samples were characterized by scanning electron microscopy, atomic force microscopy, and x-ray diffractometry. Samples of excellent optical quality were prepared. The nonlinear measurements were performed using the thermally managed eclipse Z-scan technique at 800 nm. A large value of n{sub 2}approx =10{sup -12} cm{sup 2}/W and negligible nonlinear absorption were obtained.

Hydration reactivity of crystalline and vitrified diopside under hydrothermal conditions

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

Grzeszczyk, S.; Szuba, J.

1990-07-01

Hydration reactivity of diopside in both the crystalline and amorphous (glassy) phase was studied under hydrothermal conditions. Samples were treated in an autoclave at 200{degrees}C in saturated vapor for 24 and 72 h. The progress of hydration was determined by X-ray powder diffractometry and IR spectroscopy. Results indicate that crystalline diopside possessed poor hydraulic activity. However, once vitrified it proved to be much more reactive. The principal hydration products found for the glassy diopside after 24 and 72 h of treatment were calcium silicate hydrate (xonotlite) and magnesium silicate hydrates (chrysotile and tremolite).

Synthesis and characterization of Ru-Ti[sub 4]O[sub 7] microelectrode arrays

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

He, L.; Franzen, H.F.; Vitt, J.E.

1994-04-01

A synthesis is described for Ru microelectrode arrays within a conductive Ti[sub 4]O[sub 7] ceramic matrix. Data obtained by X-ray diffractometry and scanning electron microscopy are consistent with the existence of heterogeneous mixtures of Ru particles (ca. 0.8 [mu]m diam) within the Ti[sub 4]O[sub 7] matrices. No mixed metal oxides or other new compounds are detected. Rotated disk electrodes (RDEs) constructed from the Ru-Ti[sub 4]O[sub 7] materials are compared on the basis of their voltammetric response for the oxidations of I[sup [minus

Functionalization of 2D macroporous silicon under the high-pressure oxidation

NASA Astrophysics Data System (ADS)

Karachevtseva, L.; Kartel, M.; Kladko, V.; Gudymenko, O.; Bo, Wang; Bratus, V.; Lytvynenko, O.; Onyshchenko, V.; Stronska, O.

2018-03-01

Addition functionalization after high-pressure oxidation of 2D macroporous silicon structures is evaluated. X-ray diffractometry indicates formation of orthorhombic SiO2 phase on macroporous silicon at oxide thickness of 800-1200 nm due to cylindrical symmetry of macropores and high thermal expansion coefficient of SiO2. Pb center concentration grows with the splitting energy of LO- and TO-phonons and SiO2 thickness in oxidized macroporous silicon structures. This increase EPR signal amplitude and GHz radiation absorption and is promising for development of high-frequency devices and electronically controlled elements.

Structural and mechanical behaviour of LLDPE/HNT nanocomposite films

NASA Astrophysics Data System (ADS)

Čermák, M.; Kadlec, P.; Šutta, P.; Polanský, R.

2016-03-01

The paper briefly describes structural and mechanical influences of Halloysite nanotubes (HNT) in different level of fulfilment (0, 1, 3, 7 wt%) in the LLDPE commonly used in the cable industry. The influence of HNT on the polymer has been observed and evaluated through the average crystallite size and the micro- deformation by X-Ray diffractometry and the imaging of SEM. Despite the certain inter-phase tension between the polymer and HNT, the influence on the mechanical and combustion behaviour was observed. Measurement showed a higher content of agglomerates in the sample with 7 wt% HNT fulfilment.

Study on different characteristics of doped tri calcium phosphate at different sintering temperatures

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

Samanta, Sujan Krishna, E-mail: itssujan@rediffmail.com; Chanda, Abhijit, E-mail: abhijitchanda.biomed@gmail.com

2016-04-13

Pure β-tricalcium phosphate (β-TCP), Zn-doped (3wt %) β-TCP and Mg- doped (3wt %) β-TCP samples were prepared by using a wet chemical precipitation synthesis technique, followed by calcination at 800 °C in air. The developed materials were subjected to sintering at different temperatures. Density and porosity were compared. The X-ray diffractometry (XRD) and Fourier-transformed infrared (FTIR) spectrometer were used to examine the changes in crystalline phases and presence of functional groups of TCP ceramics. The scanning electron microscopy (SEM) was used to study the pore formation, pore size, grain size.

Atomic force microscope studies of fullerene films - Highly stable C60 fcc (311) free surfaces

NASA Technical Reports Server (NTRS)

Snyder, Eric J.; Tong, William M.; Williams, R. S.; Anz, Samir J.; Anderson, Mark S.

1991-01-01

Atomic force microscopy and X-ray diffractometry were used to study 1500 A-thick films of pure C60 grown by sublimation in ultrahigh vacuum onto a CaF2 (111) substrte. Topographs of the films did not reveal the expected close-packed structures, but they showed instead large regions that correspond to a face-centered cubic (311) surface and distortions of this surface. The open (311) structure may have a relatively low free energy because the low packing density contributes to a high entropy of the exposed surface.

Structure of chitosan gels mineralized by sorption

NASA Astrophysics Data System (ADS)

Modrzejewska, Z.; Skwarczyńska, A.; Douglas, T. E. L.; Biniaś, D.; Maniukiewicz, W.; Sielski, J.

2015-10-01

The paper presents the structural studies of mineralized chitosan hydrogels. Hydrogels produced by using sodium beta-glycerophosphate (Na-β-GP) as a neutralizing agent. Mineralization was performed method "post loading", which consisted in sorption to the gels structure Ca ions. In order to obtain - in the structure of gels - compounds similar to the hydroxyapatites present naturally in bone tissue, gels after sorption were modified in: pH 7 buffer and sodium hydrogen phosphate. In order to determine the structural properties of the gels, the following methods were used: infrared spectroscopy with Fourier transformation, FTIR, X-ray diffractometry, XRD, scanning electron microscopy, SEM.

Characterization of calcium crystals in Abelia using x-ray diffraction and electron microscopes

USDA-ARS?s Scientific Manuscript database

Localization, chemical composition, and morphology of calcium crystals in leaves and stems of Abelia mosanensis and A. ×grandiflora were analyzed with a variable pressure scanning electron microscope (VP-SEM) equipped with an X-ray diffraction system, low temperature SEM (LT-SEM) and a transmission ...

Energetic Materials for Bio-Agent Destruction

DTIC Science & Technology

2017-03-01

Delocalization of electrons in 4 The structure of 5 was obtained by X-ray single crystal crystallography . The crystallographic data are summarized in...4 22.2 49.6 - - 8.36 5 18.8 41.7 - - 5.07 The structure of 5 was obtained by X-ray single crystal crystallography . The

New crystal spectrograph designs and their application to plasma diagnostics (invited)

NASA Astrophysics Data System (ADS)

Förster, E.; Gäbel, K.; Uschmann, I.

1992-10-01

A special crystal monolith was fabricated for absolute measurements of x-ray wavelength. It consists of two flat quartz plates, accurately cut relative to reflecting net planes, with a fixed distance between them. Absolute wavelengths (i.e., without use of reference lines) of L-shell laser produced spectra of Cu, Ge, As, etc. have been measured in the 7.5-8.5 Å with an accuracy of Δλ/λ=10-5. Our Johann type x-ray spectrometer with a cylindrically bent quartz has been used to reveal line coincidences necessary for photopumping processes. In this scheme source-size influences are smaller, therefore, line profiles have been measured at a spectrometer resolution better than 5000. Because of its focusing in the sagittal plane, a von Hámos type x-ray spectrometer has been used to detect the small x-ray emission of subpicosecond laser-produced plasmas (E=2 mJ, t=100 fs). X-ray spectra of Al both Kα, Kβ lines and Heα-resonance line with its satellites. Finally, a multichannel x-ray microscope has been designed and fabricated. It consists of several two-dimensionally bent crystals where each of them images one x-ray line emitted by a laser-produced plasma. The spatial resolution of x-ray line images is about 5 μm, and the width of the spectral ranges is Δλ/λ=10-4 to 10-2. Thus, the spatial distribution of ions radiating in selected x-ray lines have been found being of interest in the study of population inversions.

Simulation Studies of the X-Ray Free-Electron Laser Oscillator

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

Lindberg, R. R.; Shyd'ko, Y.; Kim, K.-J

Simulations of the x-ray free-electron laser (FEL) oscillator are presented that include transverse effects and realistic Bragg crystal properties with the two-dimensional code GINGER. In the present cases considered the radiation divergence is much narrower than the crystal acceptance, and the numerical algorithm can be simplified by ignoring the finite angular bandwidth of the crystal. In this regime GINGER shows that the saturated x-ray pulses have 109 photons and are nearly Fourier-limited with peak powers in excess of 1 MW. Wealso include preliminary results for a four-mirror cavity that can be tuned in wavelength over a few percent, with futuremore » plans to incorporate the full transverse response of the Bragg crystals into GINGER to more accurately model this tunable source.« less

Homogeneity of CdZnTe detectors

NASA Astrophysics Data System (ADS)

Hermon, H.; Schieber, M.; James, R. B.; Lund, J.; Antolak, A. J.; Morse, D. H.; Kolesnikov, N. N. P.; Ivanov, Y. N.; Goorsky, M. S.; Yoon, H.; Toney, J.; Schlesinger, T. E.

1998-02-01

We describe the current state of nuclear radiation detectors produced from single crystals of Cd 1- xZn xTe(CZT), with 0.04 < x < 0.4, grown by the vertical high pressure Bridgman (VHPB) method. The crystals investigated were grown commercially both in the USA and at the Institute of Solid State Physics, Chernogolska, Russia. The CZT was evaluated by Sandia National Laboratories and the UCLA and CMU groups using proton-induced X-ray emission (PIXE), X-ray diffraction (XRD), photoluminescence (PL), infrared (IR) transmission microscopy, leakage current measurements and response to nuclear radiation. We discuss the homogeneity of the various CZT crystals based on the results from these measurement techniques.

Purification, crystallization and preliminary X-ray diffraction studies of UDP-N-acetylglucosamine pyrophosphorylase from Candida albicans

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

Maruyama, Daisuke; Nishitani, Yuichi; Nonaka, Tsuyoshi

2006-12-01

UDP-N-acetylglucosamine pyrophosphorylase was purified and crystallized and X-ray diffraction data were collected to 2.3 Å resolution. UDP-N-acetylglucosamine pyrophosphorylase (UAP) is an essential enzyme in the synthesis of UDP-N-acetylglucosamine. UAP from Candida albicans was purified and crystallized by the sitting-drop vapour-diffusion method. The crystals of the substrate and product complexes both diffract X-rays to beyond 2.3 Å resolution using synchrotron radiation. The crystals of the substrate complex belong to the triclinic space group P1, with unit-cell parameters a = 47.77, b = 62.89, c = 90.60 Å, α = 90.01, β = 97.72, γ = 92.88°, whereas those of the productmore » complex belong to the orthorhombic space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 61.95, b = 90.87, c = 94.88 Å.« less

Crystallization and preliminary X-ray diffraction study of recombinant ribokinase from Thermus Species 2.9

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

Abramchik, Yu. A.; Timofeev, V. I., E-mail: tostars@mail.ru; Muravieva, T. I.

2016-11-15

Ribokinase from a thermophilic strain of Thermus species 2.9 belonging to the carbohydrate ribokinase family (EC 2.7.1.15) was isolated, purified, and crystallized. The crystallization conditions were found by the vapor-diffusion technique and were then optimized to apply the capillary counter-diffusion technique. The X-ray diffraction data set was collected from the crystals, which were grown by the counter-diffusion technique, at the SPring-8 synchrotron radiation facility to 2.87 Å resolution. The crystals belong to sp. gr. P12{sub 1}1 and have the following unit-cell parameters: a = 81.613 Å, b = 156.132 Å, c = 87.714 Å, α = γ = 90°, βmore » = 103.819°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the protein by the molecular-replacement method.« less

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

NASA Astrophysics Data System (ADS)

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

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

X-ray absorption fine structure (XAFS) spectroscopy using synchrotron radiation

NASA Astrophysics Data System (ADS)

Shrivastava, B. D.

2012-05-01

The X-ray absorption fine structure (XAFS) spectra are best recorded when a highly intense beam of X-rays from a synchrotron is used along with a good resolution double crystal or curved crystal spectrometer and detectors like ionization chambers, scintillation counters, solid state detectors etc. Several synchrotrons around the world have X-ray beamlines dedicated specifically to XAFS spectroscopy. Fortunately, the Indian synchrotron (Indus-2) at Raja Ramanna Centre for Advanced Technology (RRCAT) at Indore has started operation. A dispersive type EXAFS beamline called BL-8 has been commissioned at this synchrotron and another beamline having double crystal monochromator (DCM) is going to be commissioned shortly. In Indian context, in order that more research workers use these beamlines, the study of XAFS spectroscopy using synchrotron radiation becomes important. In the present work some of the works done by our group on XAFS spectroscopy using synchrotron radiation have been described.

Pink-beam serial crystallography

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

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

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

Pink-beam serial crystallography

DOE PAGES

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

2017-11-03

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

Increasing dissolution of trospium chloride by co-crystallization with urea

NASA Astrophysics Data System (ADS)

Skořepová, Eliška; Hušák, Michal; Čejka, Jan; Zámostný, Petr; Kratochvíl, Bohumil

2014-08-01

The search for various solid forms of an active pharmaceutical ingredient (API) is an important step in drug development. Our aim was to prepare co-crystals of trospium chloride, an anticholinergic drug used for the treatment of incontinence, and to investigate if they have advantageous properties for drug formulation. Phase identification was done by powder X-ray diffraction and single-crystal X-ray diffraction. The chemical composition was verified by solution NMR and the dissolution rate of the prepared phases was studied by IDR (intrinsic dissolution rate). For further analysis of phase stability and transitions, combined thermal analysis and temperature-resolved X-ray powder diffraction were used. Urea was selected as a co-crystallization partner. Trospium chloride urea (1:1) co-crystal was prepared by a solvent evaporation. From single-crystal data, the co-crystal structure was solved in a space group P21/c and compared to previously published structures of trospium chloride. Intrinsic dissolution rate revealed that the co-crystal dissolves 32% faster than pure API. However, its low thermal and pressure stability makes it a challenging choice for the final drug formulation.

Purification, crystallization and preliminary X-ray diffraction of the N-terminal calmodulin-like domain of the human mitochondrial ATP-Mg/P{sub i} carrier SCaMC1

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

Yang, Qin, E-mail: yang@crystal.harvard.edu; Brüschweiler, Sven; Chou, James J., E-mail: yang@crystal.harvard.edu

2013-12-24

The N-terminal calmodulin-like domain of the human mitochondrial ATP-Mg/P{sub i} carrier SCaMC1 was crystallized in the presence of Ca{sup 2+}. X-ray diffraction data were collected to 2.9 Å resolution from crystals which belonged to space group P6{sub 2}22.

X-ray diffraction analysis of LiCu{sub 2}O{sub 2} crystals with additives of silver atoms

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

Sirotinkin, V. P., E-mail: irotinkin.vladimir@mail.ru; Bush, A. A.; Kamentsev, K. E.

2015-09-15

Silver-containing LiCu{sub 2}O{sub 2} crystals up to 4 × 8 × 8 mm in size were grown by the crystallization of 80(1-x)CuO · 20{sub x}AgNO{sub 3} · 20Li{sub 2}CO{sub 3} (0 ≤ x ≤ 0.5) mixture melt. According to the X-ray spectral and Rietveld X-ray diffraction data, the maximum amount of silver incorporated in the LiCu{sub 2}O{sub 2} structure is about 4 at % relative to the copper content. It was established that silver atoms occupy statistically crystallographic positions of lithium atoms. The incorporation of silver atoms is accompanied by a noticeable increase in parameter c of the LiCu{sub 2}O{submore » 2} rhombic unit cell, a slight increase in parameter a, and a slight decrease in parameter b.« less

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

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

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

2014-06-09

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

X-ray diffraction analysis of LiCu2O2 crystals with additives of silver atoms

NASA Astrophysics Data System (ADS)

Sirotinkin, V. P.; Bush, A. A.; Kamentsev, K. E.; Dau, H. S.; Yakovlev, K. A.; Tishchenko, E. A.

2015-09-01

Silver-containing LiCu2O2 crystals up to 4 × 8 × 8 mm in size were grown by the crystallization of 80(1- x)CuO · 20 x AgNO3 · 20Li2CO3 (0 ≤ х ≤ 0.5) mixture melt. According to the X-ray spectral and Rietveld X-ray diffraction data, the maximum amount of silver incorporated in the LiCu2O2 structure is about 4 at % relative to the copper content. It was established that silver atoms occupy statistically crystallographic positions of lithium atoms. The incorporation of silver atoms is accompanied by a noticeable increase in parameter с of the LiCu2O2 rhombic unit cell, a slight increase in parameter а, and a slight decrease in parameter b.

Experimental and theoretical investigation of the rocking curves measured for MoK{sub α} X-ray characteristic lines in the double-crystal nondispersive scheme

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

Marchenkov, N. V., E-mail: marchenkov@ns.crys.ras.ru; Chukhovskii, F. N.; Blagov, A. E.

2015-03-15

The rocking curves (RCs) for MoK{sub α1} and MoK{sub α2} characteristic X-ray lines have been experimentally and theoretically studied in the nondispersive scheme of an X-ray double-crystal TPC-K diffractometer. The results of measurements and theoretical calculations of double-crystal RCs for characteristic X-rays from tubes with a molybdenum anode and different widths of slits show that a decrease in the slit width leads to an increase in the relative contribution of the MoK{sub α2}-line RC in comparison with the intensity of the tails of the MoK{sub α1}-line RC. It is shown that the second peak of the MoK{sub α2} line becomesmore » increasingly pronounced in the tail of the MoK{sub α1}-line RC with a decrease in the slit width. Two plane-parallel Si plates (input faces (110), diffraction vector h 〈220〉) were used as a monochromator crystal and a sample. The results of measuring double-crystal RCs are in good agreement with theoretical calculations.« less

The luminescence characteristics of CsI(Na) crystal under α and X/γ excitation

NASA Astrophysics Data System (ADS)

Liu, Jinliang; Liu, Fang; Ouyang, Xiaoping; Liu, Bin; Chen, Liang; Ruan, Jinlu; Zhang, Zhongbing; Liu, Jun

2013-01-01

In this paper, we study the effective decay time characteristic of CsI(Na) crystal under 239Pu alpha particle and 137Cs gamma-ray excitation using a single photon counting decay time measurement system. The measurement system employs a silicon optical fiber to couple and transit single photon. The slow decay time component of CsI(Na) crystal is 460-550 ns. We observe a 15 ns fast decay component under alpha particle excitation. In addition, we find that the primary stage of the falling edge in the decay time curve is non-exponential and drops rapidly when CsI(Na) crystal is excited by 239Pu alpha particles. Since the high density of self-trapped-excitons (STEs) is produced in alpha particle excitation process, we propose that the fast falling edge is corresponding to the quenching process of STEs which transit with non-radiation in the case of high excitation density. To prove this proposal, we excited the CsI(Na) crystal with sub-nanosecond intensive pulsed X-ray radiation. Our X-ray impinging results show that the fast falling edge also exists under low energy (average 100 keV) bremsstrahlung X-ray excitation.

A Newly Designed Microspectrofluorometer for Kinetic Studies on Protein Crystals in Combination with X-Ray Diffraction

PubMed Central

Klink, Björn U.; Goody, Roger S.; Scheidig, Axel J.

2006-01-01

We present a new design for a fluorescence microspectrophotometer for use in kinetic crystallography in combination with x-ray diffraction experiments. The FLUMIX device (Fluorescence spectroscopy to monitor intermediates in x-ray crystallography) is built for 0° fluorescence detection, which has several advantages in comparison to a conventional fluorometer with 90° design. Due to the reduced spatial requirements and the need for only one objective, the system is highly versatile, easy to handle, and can be used for many different applications. In combination with a conventional stereomicroscope, fluorescence measurements or reaction initiation can be performed directly in a hanging drop crystallization setup. The FLUMIX device can be combined with most x-ray sources, normally without the need of a specialized mechanical support. As a biological model system, we have used H-Ras p21 with an artificially introduced photo-labile GTP precursor (caged GTP) and a covalently attached fluorophore (IANBD amide). Using the FLUMIX system, detailed information about the state of photolyzed crystals of the modified H-Ras p21 (p21(mod)) could be obtained. Measurements in combination with a synchrotron beamline showed significant fluorescence changes in p21(mod) crystals even within a few seconds of x-ray exposure at 100 K. PMID:16698776

A seven-crystal Johann-type hard x-ray spectrometer at the Stanford Synchrotron Radiation Lightsource

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

Sokaras, D.; Weng, T.-C.; Nordlund, D.

2013-05-15

We present a multicrystal Johann-type hard x-ray spectrometer ({approx}5-18 keV) recently developed, installed, and operated at the Stanford Synchrotron Radiation Lightsource. The instrument is set at the wiggler beamline 6-2 equipped with two liquid nitrogen cooled monochromators - Si(111) and Si(311) - as well as collimating and focusing optics. The spectrometer consists of seven spherically bent crystal analyzers placed on intersecting vertical Rowland circles of 1 m of diameter. The spectrometer is scanned vertically capturing an extended backscattering Bragg angular range (88 Degree-Sign -74 Degree-Sign ) while maintaining all crystals on the Rowland circle trace. The instrument operates in atmosphericmore » pressure by means of a helium bag and when all the seven crystals are used (100 mm of projected diameter each), has a solid angle of about 0.45% of 4{pi} sr. The typical resolving power is in the order of (E/{Delta}E){approx}10 000. The spectrometer's high detection efficiency combined with the beamline 6-2 characteristics permits routine studies of x-ray emission, high energy resolution fluorescence detected x-ray absorption and resonant inelastic x-ray scattering of very diluted samples as well as implementation of demanding in situ environments.« less

Diamond drumhead crystals for X-ray optics applications

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

Kolodziej, Tomasz; Vodnala, Preeti; Terentyev, Sergey

2016-07-14

Thin (<50 µm) and flawless diamond single crystals are essential for the realization of numerous advanced X-ray optical devices at synchrotron radiation and free-electron laser facilities. The fabrication and handling of such ultra-thin components without introducing crystal damage and strain is a challenge. Drumhead crystals, monolithic crystal structures composed of a thin membrane furnished with a surrounding solid collar, are a solution ensuring mechanically stable strain-free mounting of the membranes with efficient thermal transport. Diamond, being one of the hardest and most chemically inert materials, poses significant difficulties in fabrication. Reported here is the successful manufacture of diamond drumhead crystalsmore » in the [100] orientation using picosecond laser milling. Subsequent high-temperature treatment appears to be crucial for the membranes to become defect free and unstrained, as revealed by X-ray topography on examples of drumhead crystals with a 26 µm thick (1 mm in diameter) and a 47 µm thick (1.5 × 2.5 mm) membrane.« less

Crystallization and preliminary X-ray analysis of gene product 44 from bacteriophage Mu

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

Kondou, Youhei; Faculty of Pharmaceutical Sciences, Toyama Medical and Pharmaceutical University, Toyama; Kitazawa, Daisuke

2005-01-01

Bacteriophage Mu baseplate protein gene product 44 was crystallized. The crystal belongs to space group R3, with unit-cell parameters a = b = 126.6, c = 64.2 Å. Bacteriophage Mu baseplate protein gene product 44 (gp44) is an essential protein required for the assembly of viable phages. To investigate the roles of gp44 in baseplate assembly and infection, gp44 was crystallized at pH 6.0 in the presence of 20% 2-methyl-2,4-pentanediol. The crystals belong to space group R3, with unit-cell parameters a = b = 127.47, c = 63.97 Å. The crystals diffract X-rays to at least 2.1 Å resolution andmore » are stable in the X-ray beam and are therefore appropriate for structure determination. Native data have been collected to 2.1 Å resolution using a DIP6040 image-plate system at beamline BL44XU at the SPring-8 facility in Japan.« less

Imaging crystal spectrometer for high-resolution x-ray measurements on electron beam ion traps and tokamaks

DOE PAGES

Beiersdorfer, P.; Magee, E. W.; Hell, N.; ...

2016-09-09

Here, we describe a crystal spectrometer implemented on the Livermore electron beam ion traps that employ two spherically bent quartz crystals and a cryogenically cooled back-illuminated charge-coupled device detector to measure x rays with a nominal resolving power of λ/Δλ ≥ 10 000. Its focusing properties allow us to record x rays either with the plane of dispersion perpendicular or parallel to the electron beam and, thus, to preferentially select one of the two linear x-ray polarization components. Moreover, by choice of dispersion plane and focussing conditions, we use the instrument either to image the distribution of the ions withinmore » the 2 cm long trap region, or to concentrate x rays of a given energy to a point on the detector, which optimizes the signal-to-noise ratio. We demonstrate the operation and utility of the new instrument by presenting spectra of Mo 34+, which prepares the instrument for use as a core impurity diagnostic on the NSTX-U spherical torus and other magnetic fusion devices that employ molybdenum as plasma facing components.« less

Charge-Transfer Analysis of 2p3d Resonant Inelastic X-ray Scattering of Cobalt Sulfide and Halides

PubMed Central

2017-01-01

We show that with 2p3d resonant inelastic X-ray scattering (RIXS) we can accurately determine the charge-transfer parameters of CoF2, CoCl2, CoBr2, and CoS. The 160 meV resolution RIXS results are compared with charge-transfer multiplet calculations. The improved resolution and the direct observation of the crystal field and charge-transfer excitations allow the determination of more accurate parameters than could be derived from X-ray absorption and X-ray photoemission, both limited in resolution by their lifetime broadening. We derive the crystal field and charge-transfer parameters of the Co2+ ions, which provides the nature of the ground state of the Co2+ ions with respect to symmetry and hybridization. In addition, the increased spectral resolution allows the more accurate determination of the atomic Slater integrals. The results show that the crystal field energy decreases with increasing ligand covalency. The L2 edge RIXS spectra show that the intensity of the (Coster–Kronig induced) nonresonant X-ray emission is a measure of ligand covalency. PMID:29170686

A multi-dataset data-collection strategy produces better diffraction data

PubMed Central

Liu, Zhi-Jie; Chen, Lirong; Wu, Dong; Ding, Wei; Zhang, Hua; Zhou, Weihong; Fu, Zheng-Qing; Wang, Bi-Cheng

2011-01-01

A multi-dataset (MDS) data-collection strategy is proposed and analyzed for macromolecular crystal diffraction data acquisition. The theoretical analysis indicated that the MDS strategy can reduce the standard deviation (background noise) of diffraction data compared with the commonly used single-dataset strategy for a fixed X-ray dose. In order to validate the hypothesis experimentally, a data-quality evaluation process, termed a readiness test of the X-ray data-collection system, was developed. The anomalous signals of sulfur atoms in zinc-free insulin crystals were used as the probe to differentiate the quality of data collected using different data-collection strategies. The data-collection results using home-laboratory-based rotating-anode X-ray and synchrotron X-ray systems indicate that the diffraction data collected with the MDS strategy contain more accurate anomalous signals from sulfur atoms than the data collected with a regular data-collection strategy. In addition, the MDS strategy offered more advantages with respect to radiation-damage-sensitive crystals and better usage of rotating-anode as well as synchrotron X-rays. PMID:22011470

Microgravity

NASA Image and Video Library

1999-04-21

University of Alabama engineer Stacey Giles briefs NASA astronaut Dr. Bornie Dunbar about the design and capabilities of the X-ray Crystallography Facility under development at the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, AL, April 21, 1999. The X-ray Crystallography Facility is designed to speed the collection of protein structure information from crystals grown aboard the International Space Station. By measuring and mapping the protein crystal structure in space, researchers will avoid exposing the delicate crystals to the rigors of space travel and make important research data available to scientists much faster. The X-ray Crystallography facility is being designed and developed by the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, a NASA Commercial Space Center.

Microgravity

NASA Image and Video Library

1999-04-21

University of Alabama engineer Lance Weiss briefs NASA astronaut Dr. Bornie Dunbar about the design and capabilities of the X-ray Crystallography Facility under development at the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, AL, April 21, 1999. The X-ray Crystallography Facility is designed to speed the collection of protein structure information from crystals grown aboard the International Space Station. By measuring and mapping the protein crystal structure in space, researchers will avoid exposing the delicate crystals to the rigors of space travel and make important research data available to scientists much faster. The X-ray Crystallography facility is being designed and developed by the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, a NASA Commercial Space Center.

Development of an X-ray prism for a combined diffraction enhanced imaging and fluorescence imaging system

NASA Astrophysics Data System (ADS)

Bewer, Brian E.

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These X-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing a large change in intensity for a small angle change introduced by the X-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultra small angle X-ray scattering (USAXS) contrast thus improving visualization and extending the utility of X-ray imaging. To improve on the current DEI technique this body of work describes the design of an X-ray prism (XRP) included in the imaging system which allows the analyzer crystal to be aligned anywhere on the rocking curve without moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from muradians for direct mechanical movement of the analyzer crystal to milliradian control for movement the XRP angle. In addition to using an XRP for the traditional DEI acquisition method of two scans on opposite sides of the rocking curve preliminary tests will be presented showing the potential of using an XRP to scan quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single fast measurement thus removing the occurrence of motion artifacts for each point or line used during a scan. The XRP design is also intended to be compatible with combined imaging systems where more than one technique is used to investigate a sample. Candidates for complimentary techniques are investigated and measurements from a combined X-ray imaging system are presented.

Synthesis, crystal structure and characterization of a new organic-inorganic hybrid material 4-(ammonium methyl) pipyridinium hexachloro stanate (II) trihydrate

NASA Astrophysics Data System (ADS)

Lassoued, Mohamed Saber; Abdelbaky, Mohammed S. M.; Lassoued, Abdelmajid; Ammar, Salah; Gadri, Abdellatif; Ben Salah, Abdelhamid; García-Granda, Santiago

2018-03-01

The present paper undertakes the study of (C6H16N2) SnCl6·3H2O which is a new hybrid compound. It was prepared and characterized by single crystal X-ray diffraction, X-ray powder, Hirshfeld surface, Spectroscopy measurement, thermal study and photoluminescence properties. The single crystal X-ray diffraction studies revealed that the compound crystallizes in monoclinic Cc space group with cell parameters a = 8.3309(9) Å, b = 22.956(2) Å, c = 9.8381(9) Å, β = 101.334(9) ° and Z = 4. The atomic arrangement shows an alternation of organic and inorganic entities. The cohesion between these entities is performed via Nsbnd H⋯Cl, Nsbnd H⋯O, Osbnd H⋯Cl and Osbnd H⋯O hydrogen bonding to form a three-dimensional network. Hirshfeld surface analysis was used to investigate intermolecular interactions, as well 2D finger plots were conducted to reveal the contribution of these interactions in the crystal structure quantitatively. The X-ray powder is in agreement with the X-ray structure. Scanning electron microscope (SEM) was carried out. Furthermore, the room temperature infrared (IR) spectrum of the title compound was recorded and analyzed on the basis of data found in the literature. Solid state 13C NMR spectrum shows four signals, confirming the solid state structure determined by X-ray diffraction. Besides, the thermal analysis studies were performed, but no phase transition was found in the temperature range between 30 and 450 °C. The optical and PL properties of the compound were investigated in the solid state at room temperature and exhibited three bands at 348 and 401 cm-1 and a strong fluorescence at 480 nm.

Estimation of Crystallinity of Nifedipine-Polyvinylpyrrolidone Solid Dispersion by Usage of Terahertz Time-Domain Spectroscopy and of X-Ray Powder Diffractometer.

PubMed

Takeuchi, Issei; Shimakura, Kemmaro; Kuroda, Hideki; Nakajima, Takehisa; Goto, Satoru; Makino, Kimiko

2015-12-01

Crystalline state of pharmaceutical materials is of great importance in preparation of pharmaceutics, because their physicochemical properties affect bioavailability, quality of products, therapeutic level and manufacturing process. In this study, we have estimated time-dependent changes of nifedipine in nifedipine-polyvinylpyrrolidone (PVP) solid dispersion by measuring terahertz time-domain spectroscopy (THz-TDS) and by X-ray powder diffractometry (XRPD), and compared their correlativity. Crystallinity of nifedipine-PVP solid dispersion was changed by storing the amorphous sample at 25°C-75°C and relative humidity of over 80% for 0.25-24.00 h. To compare the results of two types of measurements, we have used a general method of linear regression analysis. Crystallinities estimated using THz-TDS were plotted on the x-axis and that of XRPD were on the y-axis. From the result of the calculation, the correlativity of them was confirmed. THz-TDS has the capability of becoming the replacement of XRPD. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Luminescent properties under X-ray excitation of Ba(1-x)PbxWO4 disordered solid solution

NASA Astrophysics Data System (ADS)

Bakiz, B.; Hallaoui, A.; Taoufyq, A.; Benlhachemi, A.; Guinneton, F.; Villain, S.; Ezahri, M.; Valmalette, J.-C.; Arab, M.; Gavarri, J.-R.

2018-02-01

A series of polycrystalline barium-lead tungstate Ba1-xPbxWO4 with 0 ≤ x ≤ 1 was synthesized using a classical solid-state method with thermal treatment at 1000 °C. These materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Raman (FT-Raman) spectroscopy. X-ray diffraction profile analyses were performed using Rietveld method. These materials crystallized in the scheelite tetragonal structure and behaved as quasi ideal solid solution. Raman spectroscopy confirmed the formation of the solid solution. Structural distortions were evidenced in X-ray diffraction profiles and in vibration Raman spectra. The scanning electron microscopy experiments showed large and rounded irregular grains. Luminescence experiments were performed under X-ray excitation. The luminescence emission profiles have been interpreted in terms of four Gaussian components, with a major contribution of blue emission. The integrated intensity of luminescence reached a maximum value in the composition range x = 0.3-0.6, in relation with distortions of crystal lattice.

Kinetic products in coordination networks: ab initio X-ray powder diffraction analysis.

PubMed

Martí-Rujas, Javier; Kawano, Masaki

2013-02-19

Porous coordination networks are materials that maintain their crystal structure as molecular "guests" enter and exit their pores. They are of great research interest with applications in areas such as catalysis, gas adsorption, proton conductivity, and drug release. As with zeolite preparation, the kinetic states in coordination network preparation play a crucial role in determining the final products. Controlling the kinetic state during self-assembly of coordination networks is a fundamental aspect of developing further functionalization of this class of materials. However, unlike for zeolites, there are few structural studies reporting the kinetic products made during self-assembly of coordination networks. Synthetic routes that produce the necessary selectivity are complex. The structural knowledge obtained from X-ray crystallography has been crucial for developing rational strategies for design of organic-inorganic hybrid networks. However, despite the explosive progress in the solid-state study of coordination networks during the last 15 years, researchers still do not understand many chemical reaction processes because of the difficulties in growing single crystals suitable for X-ray diffraction: Fast precipitation can lead to kinetic (metastable) products, but in microcrystalline form, unsuitable for single crystal X-ray analysis. X-ray powder diffraction (XRPD) routinely is used to check phase purity, crystallinity, and to monitor the stability of frameworks upon guest removal/inclusion under various conditions, but rarely is used for structure elucidation. Recent advances in structure determination of microcrystalline solids from ab initio XRPD have allowed three-dimensional structure determination when single crystals are not available. Thus, ab initio XRPD structure determination is becoming a powerful method for structure determination of microcrystalline solids, including porous coordination networks. Because of the great interest across scientific disciplines in coordination networks, especially porous coordination networks, the ability to determine crystal structures when the crystals are not suitable for single crystal X-ray analysis is of paramount importance. In this Account, we report the potential of kinetic control to synthesize new coordination networks and we describe ab initio XRPD structure determination to characterize these networks' crystal structures. We describe our recent work on selective instant synthesis to yield kinetically controlled porous coordination networks. We demonstrate that instant synthesis can selectively produce metastable networks that are not possible to synthesize by conventional solution chemistry. Using kinetic products, we provide mechanistic insights into thermally induced (573-723 K) (i.e., annealing method) structural transformations in porous coordination networks as well as examples of guest exchange/inclusion reactions. Finally, we describe a memory effect that allows the transfer of structural information from kinetic precursor structures to thermally stable structures through amorphous intermediate phases. We believe that ab initio XRPD structure determination will soon be used to investigate chemical processes that lead intrinsically to microcrystalline solids, which up to now have not been fully understood due to the unavailability of single crystals. For example, only recently have researchers used single-crystal X-ray diffraction to elucidate crystal-to-crystal chemical reactions taking place in the crystalline scaffold of coordination networks. The potential of ab initio X-ray powder diffraction analysis goes beyond single-crystal-to-single-crystal processes, potentially allowing members of this field to study intriguing in situ reactions, such as reactions within pores.

Effects of rare-earth size on the electronic structure of La1−xLuxVO3.

PubMed

Chen, B; Laverock, J; Newby, D; McNulty, J F; Smith, K E; Glans, P-A; Guo, J-H; Qiao, R-M; Yang, W-L; Lees, M R; Tung, L D; Singh, R P; Balakrishnan, G

2015-03-18

The electronic structure of La(1-x)Lu(x)VO(3)(x = 0, 0.2, 0.6 and 1) single crystals has been investigated using soft x-ray absorption spectroscopy, soft x-ray emission spectroscopy, and resonant soft x-ray inelastic scattering to study the effects of rare-earth size. The x-ray absorption and emission spectra at the O K-edge present a progressive evolution with R-site cation, in agreement with local spin density approximation calculations. This evolution with R, together with the temperature dependence of the O K-edge spectra, is attributed to changes in the crystal structure of La(1-x)Lu(x)VO(3). The crystal-field dd. excitations probed by resonant inelastic x-ray scattering at the V L(3)-edge exhibit an increase in energy and enhanced intensity with the decrease of R-site ionic radius, which is mainly attributed to the increased tilting magnitude of the VO(6) octahedra. Upon cooling to ~95 K, the dd* excitations are prominently enhanced in relative Intensity, in agreement with the formation of the Jahn.Teller distortion int he orbital ordering phase. Additionally, the dd* transitions of the mixed compounds are noticeably suppressed with respect to those of the pure compounds, possibly owing to the formation of C-type orbital ordering induced by large R-site size variances.

HPHT growth and x-ray characterization of high-quality type IIa diamond.

PubMed

Burns, R C; Chumakov, A I; Connell, S H; Dube, D; Godfried, H P; Hansen, J O; Härtwig, J; Hoszowska, J; Masiello, F; Mkhonza, L; Rebak, M; Rommevaux, A; Setshedi, R; Van Vaerenbergh, P

2009-09-09

The trend in synchrotron radiation (x-rays) is towards higher brilliance. This may lead to a very high power density, of the order of hundreds of watts per square millimetre at the x-ray optical elements. These elements are, typically, windows, polarizers, filters and monochromators. The preferred material for Bragg diffracting optical elements at present is silicon, which can be grown to a very high crystal perfection and workable size as well as rather easily processed to the required surface quality. This allows x-ray optical elements to be built with a sufficient degree of lattice perfection and crystal processing that they may preserve transversal coherence in the x-ray beam. This is important for the new techniques which include phase-sensitive imaging experiments like holo-tomography, x-ray photon correlation spectroscopy, coherent diffraction imaging and nanofocusing. Diamond has a lower absorption coefficient than silicon, a better thermal conductivity and lower thermal expansion coefficient which would make it the preferred material if the crystal perfection (bulk and surface) could be improved. Synthetic HPHT-grown (high pressure, high temperature) type Ib material can readily be produced in the necessary sizes of 4-8 mm square and with a nitrogen content of typically a few hundred parts per million. This material has applications in the less demanding roles such as phase plates: however, in a coherence-preserving beamline, where all elements must be of the same high quality, its quality is far from sufficient. Advances in HPHT synthesis methods have allowed the growth of type IIa diamond crystals of the same size as type Ib, but with substantially lower nitrogen content. Characterization of this high purity type IIa material has been carried out with the result that the crystalline (bulk) perfection of some of the HPHT-grown materials is approaching the quality required for the more demanding applications such as imaging applications and imaging applications with coherence preservation. The targets for further development of the type IIa diamond are size, crystal perfection, as measured by the techniques of white beam and monochromatic x-ray diffraction imaging (historically called x-ray topography), and also surface quality. Diamond plates extracted from the cubic growth sector furthest from the seed of the new low strain material produces no measurable broadening of the x-ray rocking curve width. One measures essentially the crystal reflectivity as defined by the intrinsic reflectivity curve (Darwin curve) width of a perfect crystal. In these cases the more sensitive technique of plane wave topography has been used to establish a local upper limit of the strain at the level of an 'effective misorientation' of 10(-7) rad.

A United Effort for Crystal Growth, Neutron Scattering, and X-ray Scattering Studies of Novel Correlated Electron Materials

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

Lee, Young S.

2015-02-12

The research accomplishments during the award involved experimental studies of correlated electron systems and quantum magnetism. The techniques of crystal growth, neutron scattering, x-ray scattering, and thermodynamic & transport measurements were employed, and graduate students and postdoctoral research associates were trained in these techniques.

X-Ray Crystallography Reagent

NASA Technical Reports Server (NTRS)

Morrison, Dennis R. (Inventor); Mosier, Benjamin (Inventor)

2003-01-01

Microcapsules prepared by encapsulating an aqueous solution of a protein, drug or other bioactive substance inside a semi-permeable membrane by are disclosed. The microcapsules are formed by interfacial coacervation under conditions where the shear forces are limited to 0-100 dynes per square centimeter at the interface. By placing the microcapsules in a high osmotic dewatering solution. the protein solution is gradually made saturated and then supersaturated. and the controlled nucleation and crystallization of the protein is achieved. The crystal-filled microcapsules prepared by this method can be conveniently harvested and stored while keeping the encapsulated crystals in essentially pristine condition due to the rugged. protective membrane. Because the membrane components themselves are x-ray transparent, large crystal-containing microcapsules can be individually selected, mounted in x-ray capillary tubes and subjected to high energy x-ray diffraction studies to determine the 3-D smucture of the protein molecules. Certain embodiments of the microcapsules of the invention have composite polymeric outer membranes which are somewhat elastic, water insoluble, permeable only to water, salts, and low molecular weight molecules and are structurally stable in fluid shear forces typically encountered in the human vascular system.

Nanorelief of the natural cleavage surface of triglycine sulphate crystals with substitutional and interstitial impurities

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

Belugina, N. V.; Gainutdinov, R. V.; Tolstikhina, A. L., E-mail: alla@ns.crys.ras.ru

2011-11-15

Ferroelectric triglycine sulphate crystals (TGS) with substitutional (LADTGS+ADP, DTGS) and interstitial (Cr) impurities have been studied by atomic-force microscopy, X-ray diffraction, and X-ray fluorescence. The nanorelief parameters of the mirror cleavage TGS(010) surface have been measured with a high accuracy. A correlation between the crystal defect density in the bulk and the cleavage surface nanorelief is revealed at the submicrometer level.

Single-drop optimization of protein crystallization.

PubMed

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

2012-08-01

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

Synthesis and X-ray crystal structure determination of N- p-methylphenyl-4-benzoyl-3,4-diphenyl-2-azetidinone

NASA Astrophysics Data System (ADS)

Kabak, Mehmet; Şenöz, Hülya; Elmali, Ayhan; Adar, Vildan; Svoboda, Ingrid; Dušek, Michal; Fejfarová, Karla

2010-12-01

The title compound, C29H23NO2, has been characterized by single-crystal X-ray diffraction at two different temperatures (303 K and 120 K) and wavelengths (Mo K α and Cu K α). The non-centrosymmetric hexagonal crystal structure contains four-membered planar β-lactam ring with an unusually long C-C bond. The β-lactam ring is almost planar.

Electrochromic Properties of Tungsten Oxide Films Prepared by Reactive Sputtering

NASA Astrophysics Data System (ADS)

Kim, Min Hong; Kang, Tai Young; Jung, Yu Sup; Kim, Kyung Hwan

2013-05-01

WO3-x thin films were deposited on induim tin oxide (ITO) glass substrates with various oxygen flow ratios from 0.55 to 0.7 by the reactive facing-target sputtering method, at a power density of 4 W/cm2 and room temperature. The structural properties of the WO3-x thin films were measured by X-ray diffractometry and Raman spectral analysis. As-deposited WO3-x thin films had an amorphous structure. In the Raman spectra, WO3-x thin films exhibited two strong peaks at 770 and 950 cm-1 attributed to the vibrations of W6+-O and W6+=O bonds, respectively. The electrochemical and optical properties of WO3-x thin films were measured by cyclic voltammetry and UV/vis spectrometry. The results showed the highest charge density at an oxygen flow ratio of 0.7 and the highest transmittance in the visible range. The maximum coloration efficiency was 30.82 cm2/C at an oxygen flow ratio of 0.7.

X-ray diffraction diagnostic design for the National Ignition Facility

NASA Astrophysics Data System (ADS)

Ahmed, Maryum F.; House, Allen; Smith, R. F.; Ayers, Jay; Lamb, Zachary S.; Swift, David W.

2013-09-01

This paper describes the design considerations for Target Diffraction In-Situ (TARDIS), an x-ray diffraction diagnostic at the National Ignition Facility. A crystal sample is ramp-compressed to peak pressures between 10 and 30 Mbar and, during a pressure hold period, is probed with quasi-monochromatic x-rays emanating from a backlighter source foil. The crystal spectrography diffraction lines are recorded onto image plates. The crystal sample, filter, and image plates are packaged into one assembly, allowing for accurate and repeatable target to image plate registration. Unconverted laser light impinges upon the device, generating debris, the effects of which have been mitigated. Dimpled blast shields, high strength steel alloy, and high-z tungsten are used to shield and protect the image plates. A tapered opening was designed to provide adequate thickness of shielding materials without blocking the drive beams or x-ray source from reaching the crystal target. The high strength steel unit serves as a mount for the crystal target and x-ray source foil. A tungsten body contains the imaging components. Inside this sub-assembly, there are three image plates: a 160 degree field of view curved plate directly opposite the target opening and two flat plates for the top and bottom. A polycarbonate frame, coated with the appropriate filter material and embedded with registration features for image plate location, is inserted into the diagnostic body. The target assembly is metrologized and then the diagnostic assembly is attached.

Crystallization and preliminary X-ray analysis of gene product 44 from bacteriophage Mu

PubMed Central

Kondou, Youhei; Kitazawa, Daisuke; Takeda, Shigeki; Yamashita, Eiki; Mizuguchi, Mineyuki; Kawano, Keiichi; Tsukihara, Tomitake

2005-01-01

Bacteriophage Mu baseplate protein gene product 44 (gp44) is an essential protein required for the assembly of viable phages. To investigate the roles of gp44 in baseplate assembly and infection, gp44 was crystallized at pH 6.0 in the presence of 20% 2-methyl-2,4-pentanediol. The crystals belong to space group R3, with unit-cell parameters a = b = 127.47, c = 63.97 Å. The crystals diffract X-­rays to at least 2.1 Å resolution and are stable in the X-ray beam and are therefore appropriate for structure determination. Native data have been collected to 2.1 Å resolution using a DIP6040 image-plate system at beamline BL44XU at the SPring-8 facility in Japan. PMID:16508104

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

PubMed

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

2015-09-01

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

A new scheme for stigmatic x-ray imaging with large magnification.

PubMed

Bitter, M; Hill, K W; Delgado-Aparicio, L F; Pablant, N A; Scott, S; Jones, F; Beiersdorfer, P; Wang, E; del Rio, M Sanchez; Caughey, T A; Brunner, J

2012-10-01

This paper describes a new x-ray scheme for stigmatic imaging. The scheme consists of one convex spherically bent crystal and one concave spherically bent crystal. The radii of curvature and Bragg reflecting lattice planes of the two crystals are properly matched to eliminate the astigmatism, so that the conditions for stigmatic imaging are met for a particular wavelength. The magnification is adjustable and solely a function of the two Bragg angles or angles of incidence. Although the choice of Bragg angles is constrained by the availability of crystals, this is not a severe limitation for the imaging of plasmas, since a particular wavelength can be selected from the bremsstrahlung continuum. The working principle of this imaging scheme has been verified with visible light. Further tests with x rays are planned for the near future.

Improving a high-efficiency, gated spectrometer for x-ray Thomson scattering experiments at the National Ignition Facility.

PubMed

Döppner, T; Kraus, D; Neumayer, P; Bachmann, B; Emig, J; Falcone, R W; Fletcher, L B; Hardy, M; Kalantar, D H; Kritcher, A L; Landen, O L; Ma, T; Saunders, A M; Wood, R D

2016-11-01

We are developing x-ray Thomson scattering for applications in implosion experiments at the National Ignition Facility. In particular we have designed and fielded MACS, a high-efficiency, gated x-ray spectrometer at 7.5-10 keV [T. Döppner et al., Rev. Sci. Instrum. 85, 11D617 (2014)]. Here we report on two new Bragg crystals based on Highly Oriented Pyrolytic Graphite (HOPG), a flat crystal and a dual-section cylindrically curved crystal. We have performed in situ calibration measurements using a brass foil target, and we used the flat HOPG crystal to measure Mo K-shell emission at 18 keV in 2nd order diffraction. Such high photon energy line emission will be required to penetrate and probe ultra-high-density plasmas or plasmas of mid-Z elements.

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

PubMed Central

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

2015-01-01

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

Flux growth of high-quality CoFe 2O 4 single crystals and their characterization

NASA Astrophysics Data System (ADS)

Wang, W. H.; Ren, X.

2006-04-01

We report the growth of high-quality CoFe 2O 4 single crystals using a borax flux method. The crystals were characterized by powder X-ray diffraction, electron probe microanalysis and Raman spectroscopy. We found the crystals are flux-free and highly homogeneous in composition. X-ray rocking curves of the CoFe 2O 4 single crystals showed a full-width at half-maximum of 0.15°. The saturation magnetization of the CoFe 2O 4 single crystals was measured to be 90 emu/g or equivalently 3.65 μ B/f.u. at 5 K.

Protein Crystal Movements and Fluid Flows During Microgravity Growth

NASA Technical Reports Server (NTRS)

Boggon, Titus J.; Chayen, Naomi E.; Snell, Edward H.; Dong, Jun; Lautenschlager, Peter; Potthast, Lothar; Siddons, D. Peter; Stojanoff, Vivian; Gordon, Elspeth; Thompson, Andrew W.;

Photoluminescent properties of complex metal oxide nanopowders for gas sensing

NASA Astrophysics Data System (ADS)

Bovhyra, R. V.; Mudry, S. I.; Popovych, D. I.; Savka, S. S.; Serednytski, A. S.; Venhryn, Yu. I.

2018-03-01

This work carried out research on the features of photoluminescence of the mixed and complex metal oxide nanopowders (ZnO/TiO2, ZnO/SnO2, Zn2SiO4) in vacuum and gaseous ambient. The nanopowders were obtained using pulsed laser reactive technology. The synthesized nanoparticles were characterized by X-ray diffractometry, energy-dispersive X-ray analysis, and scanning and transmission electron microscopy analysis for their sizes, shapes and collocation. The influence of gas environment on the photoluminescence intensity was investigated. A change of ambient gas composition leads to a rather significant change in the intensity of the photoluminescence spectrum and its deformation. The most significant changes in the photoluminescent spectrum were observed for mixed ZnO/TiO2 nanopowders. This obviously is the result of a redistribution of existing centers of luminescence and the appearance of new adsorption centers of luminescence on the surface of nanopowders. The investigated nanopowders can be effectively used as sensing materials for the construction of the multi-component photoluminescent sensing matrix.

Magnetic force microscopy study of domain walls in Co{sub 2}Z ferrite

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

Qin, Lang; Verweij, Henk, E-mail: verweij.1@osu.edu

2014-03-01

Graphical abstract: - Highlights: • Hexaferrite Co{sub 2}Z is synthesized through the modified Pechini method. • Magnetic domains are observed in anisotropic Co{sub 2}Z single grain using MFM. • Observed single grain domain thickness is in good agreement with Dotsh model. - Abstract: Hexaferrite Co{sub 2}Z was synthesized through the modified Pechini method. Partially oriented samples were obtained after consolidation with uniaxial pressing and calcination/sintering at 1300 °C/1330 °C. The sample composition and morphology was identified with X-ray diffractometry (XRD) and scanning electron microscopy (SEM) with energy-dispersive X-ray spectrometry (EDS). MFM studies of the single grains revealed a domain structuremore » with 0.7 μm wide. The Co{sub 2}Z static magnetization was measured with a vibrating sample magnetometer (VSM), and was used to calculate a single grain domain with a thickness of 4.8 μm. This result is in good agreement with SEM observations of the single grain thickness.« less