Optical, electrochemical and thermal properties of Mn2+ doped CdS nanoparticles

NASA Astrophysics Data System (ADS)

Muruganandam, S.; Anbalagan, G.; Murugadoss, G.

2015-08-01

Mn2+ doped (1-5 and 10 %) CdS nanoparticles have been synthesized by the chemical precipitation method using polyvinylpyrrolidone as a capping agent. The particle size, morphology and optical properties have been studied by X-ray powder diffraction, transmission electron microscopy, UV-Visible and photoluminescence spectroscopy. Powder diffraction data have confirmed that the crystallite size is around 2-5 nm. The band gap of the nanoparticles has been calculated using UV-Visible absorption spectra. An optimum concentration, Mn2+ (3 %) has been selected by optical study. The functional groups of the capping agent have been identified by fourier transform infrared spectroscopy study. The presence of dopant (Mn2+) has been confirmed by electron paramagnetic resonance spectroscopy. Thermal properties of CdS:Mn2+ have been analyzed using thermogravimetric-differential thermal analyser. The electrochemical properties of the undoped and doped samples have been studied by cyclic voltammetry for electrode applications. In addition, magnetic properties of Mn2+ doped CdS have been studied using a vibrating sample magnetometer.

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

PubMed

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

2012-11-01

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

Growth and dielectric, mechanical, thermal and etching studies of an organic nonlinear optical L-arginine trifluoroacetate (LATF) single crystal

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

Arjunan, S.; Department of Physics, Presidency College, Chennai 600005; Mohan Kumar, R.

2008-08-04

L-arginine trifluoroacetate, an organic nonlinear optical material, has been synthesized from aqueous solution. Bulk single crystal of dimension 57 mm x 5 mm x 3 mm has been grown by temperature lowering technique. Powder X-ray diffraction studies confirmed the monoclinic structure of the grown L-arginine trifluoroacetate crystal. Linear optical property of the grown crystal has been studied by UV-vis spectrum. Dielectric response of the L-arginine trifluoroacetate crystal was analysed for different frequencies and temperatures in detail. Microhardness study on the sample reveals that the crystal possesses relatively higher hardness compared to many organic crystals. Thermal analyses confirmed that the L-argininemore » trifluoroacetate material is thermally stable upto 212 deg. C. The etching studies have been performed to assess the perfection of the L-arginine trifluoroacetate crystal. Kurtz powder second harmonic generation test confirms the nonlinear optical properties of the as-grown L-arginine trifluoroacetate crystal.« less

Synthesis, growth, structural, spectroscopic and optical studies of a new semiorganic nonlinear optical crystal: L-valine hydrochloride.

PubMed

Kirubavathi, K; Selvaraju, K; Valluvan, R; Vijayan, N; Kumararaman, S

2008-04-01

Single crystals of a new semiorganic nonlinear optical (NLO) material, L-valine hydrochloride (LVHCl), having dimensions up to 20 mm x 6 mm x 4 mm have been grown by slow evaporation solution growth technique. Single crystal X-ray diffraction studies confirm that the grown crystal belongs to the monoclinic system. The functional groups presented in the crystal were confirmed by Fourier transform infrared (FTIR) technique. Optical transmission spectrum shows very low absorption in the entire visible region. Differential thermal and thermogravimetric analyses confirmed that the crystal is stable up to 211 degrees C. The powder second harmonic generation (SHG) efficiency of LVHCl is 1.7 times efficient as potassium dihydrogen phosphate (KDP).

Studies on synthesis, growth, structural, thermal, linear and nonlinear optical properties of organic picolinium maleate single crystals.

PubMed

Pandi, P; Peramaiyan, G; Sudhahar, S; Chakkaravarthi, G; Mohan Kumar, R; Bhagavannarayana, G; Jayavel, R

2012-12-01

Picolinium maleate (PM), an organic material has been synthesised and single crystals were grown by slow evaporation technique. The structure of the grown crystal was elucidated by using single crystal X-ray diffraction analysis. PM crystal belongs to the monoclinic crystallographic system with space group P2(1)/c. The crystalline perfection of the grown crystals was analyzed by high-resolution X-ray diffraction rocking curve measurements. The presence of functional groups in PM was identified by FTIR and FT-NMR spectral analyses. Thermal behaviour and stability of picolinium maleate were studied by TGA/DTA analyses. UV-Vis spectral studies reveal that PM crystals are transparent in the wavelength region 327-1100 nm. The laser damage threshold value of PM crystal was found to be 4.3 GW/cm(2) using Nd:YAG laser. The Kurtz and Perry powder second harmonic generation technique confirms the nonlinear optical property of the grown crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

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.

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.

Air and moisture stable covalently-bonded tin(ii) coordination polymers.

PubMed

de Lima, G M; Walton, R I; Clarkson, G J; Bitzer, R S; Ardisson, J D

2018-06-05

Four covalently-bonded tin(ii) coordination polymers, (1)-(4), were hydrothermally prepared in aqueous alkaline media by the reactions of SnSO4 with 1,2,4,5-benzenetetracarboxylic acid (1), 1,3,5-benzenetricarboxylic acid (2), 4-hydroxypyridine-2,6-dicarboxylic acid (3), and 1,3,5-cyclohexanetricarboxylic acid (4). All products were structurally authenticated by single-crystal X-ray diffraction, and the number of different tin centres and their oxidation states were confirmed by 119Sn Mössbauer spectroscopy. In addition, the comparison between experimental and simulated X-ray powder diffraction patterns confirmed the authenticity of the samples. Our crystallographic results for (1)-(4) show that the Sn(ii) centres are tetracoordinated and exhibit distorted disphenoidal geometries, corroborating the presence of one stereochemically active lone electron pair at each metal site. Products (1) and (2) display bi-dimensional polymeric structures, (3) exhibits a one-dimensional architecture, whereas (4) shows a remarkable three-dimensional coordination network. Hirshfeld surface and supramolecular analyses for the repeating units of (1)-(4) were also performed in order to identify structurally important non-covalent interactions.

Nonlinear dependence of X-ray diffraction peak broadening in In x Ga1‑ x Sb epitaxial layers on GaAs substrates

NASA Astrophysics Data System (ADS)

Hoang Huynh, Sa; Ha, Minh Thien Huu; Binh Do, Huy; Nguyen, Tuan Anh; Luc, Quang Ho; Chang, Edward Yi

2018-04-01

The configuration of the interfacial misfit array at In x Ga1‑ x Sb/GaAs interfaces with different indium compositions and thicknesses grown by metalorganic chemical vapor deposition was systematically analyzed using X-ray diffraction (XRD) reciprocal space maps (RSMs). These analyses confirmed that the epilayer relaxation was mainly contributed to by the high degree of spatial correlation of the 90° misfit array (correlation factors <0.01). The anisotropic peak-broadening aspect ratio was found to have a non-linear composition dependence as well as be thickness-dependent, related to the strain relaxation of the epilayer. However, the peak-broadening behavior in each RSM scan direction had different composition and thickness dependences.

Investigations into phase effects from diffracted Gaussian beams for high-precision interferometry

NASA Astrophysics Data System (ADS)

Lodhia, Deepali

Gravitational wave detectors are a new class of observatories aiming to detect gravitational waves from cosmic sources. All-reflective interferometer configurations have been proposed for future detectors, replacing transmissive optics with diffractive elements, thereby reducing thermal issues associated with power absorption. However, diffraction gratings introduce additional phase noise, creating more stringent conditions for alignment stability, and further investigations are required into all-reflective interferometers. A suitable mathematical framework using Gaussian modes is required for analysing the alignment stability using diffraction gratings. Such a framework was created, whereby small beam displacements are modelled using a modal technique. It was confirmed that the original modal-based model does not contain the phase changes associated with grating displacements. Experimental tests verified that the phase of a diffracted Gaussian beam is independent of the beam shape. Phase effects were further examined using a rigorous time-domain simulation tool. These findings show that the perceived phase difference is based on an intrinsic change of coordinate system within the modal-based model, and that the extra phase can be added manually to the modal expansion. This thesis provides a well-tested and detailed mathematical framework that can be used to develop simulation codes to model more complex layouts of all-reflective interferometers.

A new formulation of curcumin using poly (lactic-co-glycolic acid)—polyethylene glycol diblock copolymer as carrier material

NASA Astrophysics Data System (ADS)

Phuong Tuyen Dao, Thi; Hoai Nguyen, To; To, Van Vinh; Ho, Thanh Ha; Nguyen, Tuan Anh; Chien Dang, Mau

2014-09-01

The aim of this study is to fabricate a nanoparticle formulation of curcumin using a relatively new vehicle as the matrix polymer: poly(lactic-co-glycolic acid) (PLGA)- polyethylene glycol (PEG) diblock copolymer, and to investigate the effects of the various processing parameters on the characteristics of nanoparticles (NPs). We successfully synthesized the matrix polymer of PLGA-PEG by conjugation of PLGA copolymer with a carboxylate end group to a heterobifunctional amine-PEG-methoxy using N-(3-dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide as conjugation crosslinkers. The composition of the formed product (PLGA-PEG) was characterized with 500 MHz 1H nuclear magnetic resonance (NMR). The conjugation of PLGA-PEG was confirmed using Fourier transform infrared (FTIR) spectrum study. This diblock copolymer was then used to prepare the curcumin-loaded NPs through nanoprecipitation technique. With this method, we found that the size distribution depends on the type of solvent, the concentration of polymer and the concentration of surfactant. The particle size and size distribution were measured by dynamic light scattering (DLS). Transmission electron microscope (TEM) and scanning electron microscope (SEM) were used to confirm the size, structure and morphology of the successfully prepared NPs. All of our results showed that they are spherical and quite homologous with mean diameter around of 100-300 nm. Further, we evaluated encapsulation efficiency and some characteristics of NPs through high performance liquid chromatography (HPLC) analyses, zeta-potential measurements and x-ray diffraction studies. The HPLC analyses were performed to determine the amount of curcumin entrapped in NPs. The zeta-potential measurements confirmed the stability of NPs and the successful encapsulation of curcumin within NPs and the x-ray diffraction patterns showed the disordered-crystalline phase of curcumin inside the polymeric matrix.

Syntheses, structural characterization, and DPPH radical scavenging activity of cocrystals of caffeine with 1- and 2-naphthoxyacetic acids

NASA Astrophysics Data System (ADS)

Suresh Kumar, G. S.; Seethalakshmi, P. G.; Sumathi, D.; Bhuvanesh, N.; Kumaresan, S.

2013-03-01

Caffeine:1-naphthoxyacetic acid [(caf)(1-naa)] and caffeine:2-naphthoxyacetic acid [(caf)(2-naa)] cocrystals have been synthesized and single crystals were grown by slow evaporation technique. The structures of the grown crystals were elucidated using single crystal X-ray diffraction analysis. Both the cocrystals belong to the monoclinic crystallographic system with space group P21/c, Z = 4, and α = γ = 90°, whereas β = 111.4244(18)° for [(caf)(1-naa)] and β = 109.281(6)° for [(caf)(2-naa)]. The crystal packing is predominantly stabilized by hydrogen bonding and π-π stacking interactions. The presence of unionized -COOH functional group in both the cocrystals was identified by FTIR spectral analysis. Thermal behavior and stability of both the cocrystals were studied by TGA/DTA analyses. Solvent-free formation of these cocrystals was confirmed by powder X-ray diffraction analyses. The theoretical energy of cocrystals showed that the formers have higher energy than cocrystals 1 and 2. DPPH radical scavenging activity of cocrystals 1 and 2 is slightly greater than the formers.

Investigation of La and Al substitution on the spontaneous polarization and lattice dynamics of the Pb(1-x)LaxTi(1-x)AlxO3 ceramics

NASA Astrophysics Data System (ADS)

Yadav, Arun Kumar; Verma, Anita; Kumar, Sunil; Srihari, Velaga; Sinha, A. K.; Reddy, V. Raghavendra; Liu, Shun Wei; Biring, Sajal; Sen, Somaditya

2018-03-01

The phase purity and crystal structure of Pb(1-x)LaxTi(1-x)AlxO3 (0 ≤ x ≤ 0.25) samples (synthesized via the sol-gel process) were confirmed using synchrotron x-ray powder diffraction (XRD) (wavelength, λ = 0.44573 Å). Rietveld analyses of powder x-ray diffraction data confirmed the tetragonal structure for compositions with x ≤ 0.18 and cubic structure for the sample with x = 0.25. Temperature-dependent XRD was performed to investigate the structural change from tetragonal to cubic structure phase transition. Raman spectroscopy at room temperature also confirmed this phase transition with compositions. Field emission scanning electron microscopy (FESEM) provided information about the surface morphology while an energy dispersive x-ray spectrometer attached with FESEM confirmed the chemical compositions of samples. Temperature and frequency dependent dielectric studies showed that the tetragonal to cubic phase transition decreased from 680 K to 175 K with an increase in the x from 0.03 to 0.25, respectively. This is correlated with the structural studies. Electric field dependent spontaneous polarization showed a proper ferroelectric loop for 0.06 ≤ x ≤ 0.18 belonging to a tetragonal phase, while for x ≥ 0.25, the spontaneous polarization vanishes. Bipolar strain versus electric field revealed a butterfly loop for 0.06 ≤ x ≤ 0.18 compositions. Energy storage efficiency initially increases nominally with substitution but beyond x = 0.18 enhances considerably.

Structural, Optical and Ethanol Sensing Properties of Dy-Doped SnO2 Nanoparticles

NASA Astrophysics Data System (ADS)

Shaikh, F. I.; Chikhale, L. P.; Nadargi, D. Y.; Mulla, I. S.; Suryavanshi, S. S.

2018-04-01

We report a facile co-precipitation synthesis of dysprosium (Dy3+) doped tin oxide (SnO2) thick films and their use as gas sensors. The doping percentage (Dy3+) was varied from 1 mol.% to 4 mol.% with the step of 1 mol.%. As-produced material with varying doping levels were sintered in air; and by using a screen printing technique, their thick films were developed. Prior to sensing performance investigations, the films were examined for structural, morphological and compositional properties using x-ray diffraction, a field emission scanning electron microscope, a transmission electron microscope, selected area electron diffraction, energy dispersive analysis by x-rays, Fourier transform infrared spectroscopy and Raman spectroscopic techniques. The structural analyses revealed formation of single phase nanocrystalline material with tetragonal rutile structure of SnO2. The morphological analyses confirmed the nanocrystalline porous morphology of as-developed material. Elemental analysis defined the composition of material in accordance with the doping concentration. The produced sensor material exhibited good response towards different reducing gases (acetone, ethanol, LPG, and ammonia) at different operating temperatures. The present study confirms that the Dy3+ doping in SnO2 enhances the response towards ethanol with reduction in operating temperature. Particularly, 3 mol.% Dy3+ doped sensor exhibited the highest response (˜ 92%) at an operating temperature of 300°C with better selectivity, fast response (˜ 13 s) and recovery (˜ 22 s) towards ethanol.

Synthesis, nucleation, growth, structural, spectral, thermal, linear and nonlinear optical studies of novel organic NLO crystal: 4-fluoro 4-nitrostilbene (FONS).

PubMed

Dinakaran, Paul M; Kalainathan, S

2013-03-15

A novel organic nonlinear optical material 4-fluoro 4-nitrostilbene (FONS), with molecular formula (C(14)H(10)FNO(2)) has been synthesized. Using ethyl methyl ketone as solvent, the synthesized material has been repeatedly recrystallized to minimize the impurities and good optical quality single crystals were harvested by slow evaporation method. Single crystal X-ray diffraction analysis reveals that the grown FONS crystal belongs to monoclinic system with noncentrosymmetric space group "P2(1)". The powder X-ray diffraction pattern of FONS has been recorded. Functional groups of the title compound were confirmed by FTIR and the molecular structure was confirmed by (1)HNMR. The UV-vis-NIR absorption study reveals no absorption in the visible region and the cut-off wavelength was found to be at 408 nm. Optical band gap (E(g)) of the grown crystal was found to be 3.27 eV and also the optical constants were determined. Thermal behaviour of the FONS has been studied by TGA/DTA analyses. From the mass spectrum, the ratio of compound formation of FONS was analyzed. The NLO property has been confirmed by Kurtz and Perry powder SHG technique and the SHG efficiency of FONS (262 mV) crystal was found to be 12 times greater than that of KDP (21.7 mV). Copyright © 2013 Elsevier B.V. All rights reserved.

Four new compounds from Imperata cylindrica.

PubMed

Liu, Xuan; Zhang, Bin-Feng; Yang, Li; Chou, Gui-Xin; Wang, Zheng-Tao

2014-04-01

Four new compounds, impecylone (1), deacetylimpecyloside (2), seguinoside K 4-methylether (3) and impecylenolide (4), were isolated from Imperata cylindrica along with two known compounds, impecyloside (5) and seguinoside K (6). Their structures were elucidated mainly by spectroscopic analyses including 1D- and 2D-NMR techniques, and the absolute configuration of 1 was confirmed by X-ray diffraction analysis. In calcium assay, the result indicated that compounds 1, 2, 4 and 5 cannot obviously inhibit the calcium peak value compared with the negative control, and suggested that the four compounds could not have anti-inflammatory activity.

Magnetic ground state of the multiferroic hexagonal LuFe O3

NASA Astrophysics Data System (ADS)

Suresh, Pittala; Vijaya Laxmi, K.; Bera, A. K.; Yusuf, S. M.; Chittari, Bheema Lingam; Jung, Jeil; Anil Kumar, P. S.

2018-05-01

The structural, electric, and magnetic properties of bulk hexagonal LuFe O3 are investigated. Single phase hexagonal LuFe O3 has been successfully stabilized in the bulk form without any doping by sol-gel method. The hexagonal crystal structure with P 63c m space group has been confirmed by x-ray-diffraction, neutron-diffraction, and Raman spectroscopy study at room temperature. Neutron diffraction confirms the hexagonal phase of LuFe O3 persists down to 6 K. Further, the x-ray photoelectron spectroscopy established the 3+ oxidation state of Fe ions. The temperature-dependent magnetic dc susceptibility, specific heat, and neutron-diffraction studies confirm an antiferromagnetic ordering below the Néel temperature (TN)˜130 K . Analysis of magnetic neutron-diffraction patterns reveals an in-plane (a b -plane) 120∘ antiferromagnetic structure, characterized by a propagation vector k =(0 0 0 ) with an ordered moment of 2.84 μB/F e3 + at 6 K. The 120∘ antifferomagnetic ordering is further confirmed by spin-orbit coupling density functional theory calculations. The on-site coulomb interaction (U ) and Hund's parameter (JH) on Fe atoms reproduced the neutron-diffraction Γ1 spin pattern among the Fe atoms. P -E loop measurements at room temperature confirm an intrinsic ferroelectricity of the sample with remnant polarization Pr˜0.18 μ C /c m2 . A clear anomaly in the dielectric data is observed at ˜TN revealing the presence of magnetoelectric coupling. A change in the lattice constants at TN has also been found, indicating the presence of a strong magnetoelastic coupling. Thus a coupling between lattice, electric, and magnetic degrees of freedom is established in bulk hexagonal LuFe O3 .

Cooperative interactions in dense thermal Rb vapour confined in nm-scale cells

NASA Astrophysics Data System (ADS)

Keaveney, James

Gravitational wave detectors are a new class of observatories aiming to detect gravitational waves from cosmic sources. All-reflective interferometer configurations have been proposed for future detectors, replacing transmissive optics with diffractive elements, thereby reducing thermal issues associated with power absorption. However, diffraction gratings introduce additional phase noise, creating more stringent conditions for alignment stability, and further investigations are required into all-reflective interferometers. A suitable mathematical framework using Gaussian modes is required for analysing the alignment stability using diffraction gratings. Such a framework was created, whereby small beam displacements are modelled using a modal technique. It was confirmed that the original modal-based model does not contain the phase changes associated with grating displacements. Experimental tests verified that the phase of a diffracted Gaussian beam is independent of the beam shape. Phase effects were further examined using a rigorous time-domain simulation tool. These findings show that the perceived phase difference is based on an intrinsic change of coordinate system within the modal-based model, and that the extra phase can be added manually to the modal expansion. This thesis provides a well-tested and detailed mathematical framework that can be used to develop simulation codes to model more complex layouts of all-reflective interferometers.

Synthesis, growth, structural, thermal and optical studies of pyrrolidinium-2-carboxylate-4-nitrophenol single crystals.

PubMed

Swarna Sowmya, N; Sampathkrishnan, S; Vidyalakshmi, Y; Sudhahar, S; Mohan Kumar, R

2015-06-15

Organic nonlinear optical material, pyrrolidinium-2-carboxylate-4-nitrophenol (PCN) was synthesized and single crystals were grown by slow evaporation solution growth method. Single crystal X-ray diffraction analysis confirmed the structure and lattice parameters of PCN crystals. Infrared, Raman and NMR spectral analyses were used to elucidate the functional groups present in the compound. The thermal behavior of synthesized compound was studied by thermogravimetric and differential scanning calorimetry (TG-DSC) analyses. The photoluminescence property was studied by exciting the crystal at 360 nm. The relative second harmonic generation (SHG) efficiency of grown crystal was estimated by using Nd:YAG laser with fundamental wavelength of 1,064 nm. Copyright © 2015 Elsevier B.V. All rights reserved.

Coherent X-Ray Diffraction Imaging of Chloroplasts from Cyanidioschyzon merolae by Using X-Ray Free Electron Laser.

PubMed

Takayama, Yuki; Inui, Yayoi; Sekiguchi, Yuki; Kobayashi, Amane; Oroguchi, Tomotaka; Yamamoto, Masaki; Matsunaga, Sachihiro; Nakasako, Masayoshi

2015-07-01

Coherent X-ray diffraction imaging (CXDI) is a lens-less technique for visualizing the structures of non-crystalline particles with the dimensions of submicrometer to micrometer at a resolution of several tens of nanometers. We conducted cryogenic CXDI experiments at 66 K to visualize the internal structures of frozen-hydrated chloroplasts of Cyanidioschyzon merolae using X-ray free electron laser (XFEL) as a coherent X-ray source. Chloroplast dispersed specimen disks at a number density of 7/(10×10 µm(2)) were flash-cooled with liquid ethane without staining, sectioning or chemical labeling. Chloroplasts are destroyed at atomic level immediately after the diffraction by XFEL pulses. Thus, diffraction patterns with a good signal-to-noise ratio from single chloroplasts were selected from many diffraction patterns collected through scanning specimen disks to provide fresh specimens into the irradiation area. The electron density maps of single chloroplasts projected along the direction of the incident X-ray beam were reconstructed by using the iterative phase-retrieval method and multivariate analyses. The electron density map at a resolution of 70 nm appeared as a C-shape. In addition, the fluorescence image of proteins stained with Flamingo™ dye also appeared as a C-shape as did the autofluorescence from Chl. The similar images suggest that the thylakoid membranes with an abundance of proteins distribute along the outer membranes of chloroplasts. To confirm the present results statistically, a number of projection structures must be accumulated through high-throughput data collection in the near future. Based on the results, we discuss the feasibility of XFEL-CXDI experiments in the structural analyses of cellular organelles. © The Author 2015. Published by Oxford University Press on behalf of Japanese Society of Plant Physiologists. All rights reserved. For permissions, please email: journals.permissions@oup.com.

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

NASA Astrophysics Data System (ADS)

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

2017-07-01

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

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

PubMed

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

2015-01-25

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

Synthesis and Characterization of the First Liquid Single Source Precursors for the Deposition of Ternary Chalcopyrite (CuInS2) Thin Film Materials

NASA Technical Reports Server (NTRS)

Banger, Kulbinder K.; Cowen, Jonathan; Hepp, Aloysius

2002-01-01

Molecular engineering of ternary single source precursors based on the [{PBu3}2Cu(SR')2In(SR')2] architecture have afforded the first liquid CIS ternary single source precursors (when R = Et, n-Pr), which are suitable for low temperature deposition (< 350 C). Thermogravimetric analyses (TGA) and modulated-differential scanning calorimetry (DSC) confirm their liquid phase and reduced stability. X-ray diffraction studies, energy dispersive analyzer (EDS), and scanning electron microscopy (SEM) support the formation of the single-phase chalcopyrite CuInS2 at low temperatures.

Growth, density functional theory (DFT) and spectral studies on L-2-aminobutyric acid -biologically active material

NASA Astrophysics Data System (ADS)

Usha, C.; Santhakumari, R.; Meenakshi, R.; Jayasree, R.; Bhuvaneswari, M.

2017-12-01

Single crystal of L-2-aminobutyric acid (ABA) was grown from water by slow evaporation at room temperature. The crystalline nature of the grown crystal was confirmed using powder X-ray diffraction studies. The grown crystal was subjected to FT-IR, FT-Raman, 1H NMR and 13C NMR spectral analyses to confirm the presence of functional group and molecular structure respectively. Thermal properties were investigated by thermogravimetric and differential thermal analyses. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. The electronic charge distribution and reactivity of the molecules within the crystal were studied by HOMO and LUMO analysis and the molecular electrostatic potential (MEP) of the grown crystal was performed using the B3LYP method. The anti-bacterial activities of the crystal were performed by disk diffusion method against the standard bacteria E. coli. The crystal exhibits good anti-bacterial activity. Second harmonic generation efficiency of the powdered ABA crystal was tested using Nd:YAG laser and it is found to be ∼3.3 times that of potassium dihydrogen orthophosphate.

Establishment of the structural and enhanced physicochemical properties of the cocrystal-2-benzyl amino pyridine with oxalic acid

NASA Astrophysics Data System (ADS)

Sangeetha, M.; Mathammal, R.

2017-09-01

We report on a cocrystal of 2-(benzyl amino) pyridine (BAP) with oxalic acid (OA) in the ratio 1:1. The cocrystal was synthesised and single crystals were grown under slow evaporation technique at room temperature. Single crystal X-ray diffraction (SCXRD) analysis determined the structure of the cocrystal formed and it belongs to orthorhombic system with Cc space group. It was also subjected to X-ray Powder diffraction (XRPD) to confirm the cocrystal structure. Hirshfeld surfaces and fingerprints were plotted to analyze the intermolecular interactions. Spectroscopic techniques such as FTIR, FT-Raman and NMR were carried out to identify the functional groups present in the cocrystal. The bioactivity of the cocrystal was revealed from the UV-Vis analysis. Computational Density Functional Theory (DFT) was adopted at the B3LYP/6-31+G** level to calculate the optimized geometrical parameters and the vibrational frequencies of the cocrystal. The non-linear optical property of the cocrystal was revealed from the SHG test. The different types of interactions and delocalization of charge were analysed from Natural Bond Orbital (NBO) calculations. The HOMO-LUMO energies and MEP surface maps confirmed the pharmaceutical importance of the (1:1) BAPOA cocrystal. The cocrystal has been explored for the invitro antioxidant activity and insilico molecular docking studies.

Processing and optical characterization of lead calcium titanate borosilicate glass doped with germanium

NASA Astrophysics Data System (ADS)

Gautam, C. R.; Das, Sangeeta; Gautam, S. S.; Madheshiya, Abhishek; Singh, Anod Kumar

2018-04-01

In this study, various compositions of lead calcium titanate borosilicate glass doped with a fixed amount of germanium were synthesized using the rapid melt quench technique. The amorphous nature of the synthesized glass was confirmed by X-ray diffraction and scanning electron microscopy analyses. The structural and optical properties were deduced using Raman, Fourier transform infrared (FTIR), and ultraviolet-visible (UV-Vis) spectroscopy. FTIR spectroscopy confirmed the presence of borate groups in triangular and tetrahedral coordination. Infrared and Raman analyses detected the vibrational bonds of Gesbnd Osbnd Ge, Bsbnd Osbnd Ge, Sisbnd Osbnd Ge, Sisbnd Osbnd Si, and Pbsbnd Osbnd Ge. The energy band gaps were evaluated for the prepared glass samples based on Tauc plots of the UV-Vis spectra. The calculated values of the optical band gap decreased from 2.91 to 2.85 eV as the PbO content increased from x = 0.0 to x = 0.7. Furthermore, the Urbach energy was studied based on the UV-Vis results to confirm the disordered structure of the glass. The calculated densities of the glass samples (1.5835 g/cm3 to 3.9184 g/cm3) increased as the concentration of PbO increased, whereas they decreased with the molar volume.

Microstructural studies of 35 degrees C copper Ni-Ti orthodontic wire and TEM confirmation of low-temperature martensite transformation.

PubMed

Brantley, William A; Guo, Wenhua; Clark, William A T; Iijima, Masahiro

2008-02-01

Previous temperature-modulated differential scanning calorimetry (TMDSC) study of nickel-titanium orthodontic wires revealed a large exothermic low-temperature peak that was attributed to transformation within martensitic NiTi. The purpose of this study was to use transmission electron microscopy (TEM) to verify this phase transformation in a clinically popular nickel-titanium wire, identify its mechanism and confirm other phase transformations found by TMDSC, and to provide detailed information about the microstructure of this wire. The 35 degrees C Copper nickel-titanium wire (Ormco) with cross-section dimensions of 0.016 in. x 0.022 in. used in the earlier TMDSC investigation was selected. Foils were prepared for TEM analyses by mechanical grinding, polishing, dimpling, ion milling and plasma cleaning. Standard bright-field and dark-field TEM images were obtained, along with convergent-beam electron diffraction patterns. A cryo-stage with the electron microscope (Phillips CM 200) permitted the specimen to be observed at -187, -45, and 50 degrees C, as well as at room temperature. Microstructures were also observed with an optical microscope and a scanning electron microscope. Room temperature microstructures had randomly oriented, elongated grains that were twinned. Electron diffraction patterns confirmed that phase transformations took place over temperature ranges previously found by TMDSC. TEM observations revealed a high dislocation density and fine-scale oxide particles, and that twinning is the mechanism for the low-temperature transformation in martensitic NiTi. TEM confirmed the low-temperature peak and other phase transformations observed by TMDSC, and revealed that twinning in martensite is the mechanism for the low-temperature peak. The high dislocation density and fine-scale oxide particles in the microstructure are the result of the wire manufacturing process.

Effect of solvents on optical band gap of silicon-doped graphene oxide

NASA Astrophysics Data System (ADS)

Tul Ain, Qura; Al-Modlej, Abeer; Alshammari, Abeer; Naeem Anjum, Muhammad

2018-03-01

The objective of this study was to determine the influence on the optical band gap when the same amount of silicon-doped graphene oxide was dissolved in three different solvents namely, distilled water, benzene, and dichloroethane. Ultraviolet-visible spectroscopy was used to analyse the optical properties of the solutions. Among all these solutions distilled water containing silicon-doped graphene oxide has the smallest optical band gap of 2.9 eV and is considered a semiconductor. Other solutions are not considered as semiconductors as they have optical band gaps greater than 4 eV. It was observed that there is an increase in the value of optical band gap of distilled water, benzene, and dichloroethane solutions indicating a rise in the insulating behaviour. In this experiment, graphene oxide was synthesised from graphite powder by modified Hummer’s method and was then doped with silicon. Synthesis and doping of graphene oxide were confirmed by various characterization techniques. Fourier transmission infrared spectroscopy was used for identification of surface functional groups. X-ray diffraction was carried out to confirm the formation of crystalline graphene oxide and silicon doped graphene oxide. In x-ray diffraction pattern, shifting of intensity peak from a 2θ value of 26.5° to 10° confirmed the synthesis of graphene oxide and various intensity peaks at different values of 2θ confirmed doping of graphene oxide with silicon. Scanning electron microscopy images indicated that graphene oxide sheets were decorated with spherical silicon nanoparticles. Energy dispersive x-ray spectroscopy showed that silicon doped graphene oxide powder contained 63.36% carbon, 34.05% oxygen, and 2.6% silicon.

ent-Kaurane Diterpenoids with Neuroprotective Properties from Corn Silk ( Zea mays).

PubMed

Qi, Xiao-Li; Zhang, Ying-Ying; Zhao, Peng; Zhou, Le; Wang, Xiao-Bo; Huang, Xiao-Xiao; Lin, Bin; Song, Shao-Jiang

2018-05-25

Thirteen new ent-kaurane diterpenoids, stigmaydenes A-M (1-13), together with two known compounds (14, 15), were isolated from the crude extract of corn silk ( Zea mays). The structures of the compounds were confirmed by comprehensive spectroscopic analyses. The absolute configuration of compound 1 was defined by single-crystal X-ray diffraction. The absolute configurations of the compounds were also confirmed by comparison of experimental and calculated specific rotations. The compounds were evaluated for their neuroprotective effects against H 2 O 2 -induced SH-SY5Y cell injury, and compound 8 was active at 100 μM, as determined by flow cytometry (annexin V-FITC/PI staining) and Hoechst 33258 staining. The results suggested that compound 8 could protect neuronal cells from H 2 O 2 -induced injury by inhibiting apoptosis in SH-SY5Y cells.

Photocatalytic degradation of Orange G dye under solar light using nanocrystalline semiconductor metal oxide.

PubMed

Thennarasu, G; Kavithaa, S; Sivasamy, A

2011-08-01

The photocatalytic degradation of Orange G (OG) dye has been investigated using synthesised nanocrystalline ZnO as a photocatalyst and sunlight as the irradiation source. The formation of ZnO prepared from its precursor was confirmed through FT-IR and powder X-ray diffraction analyses. Surface morphology was characterised by scanning electron microscope and transmission electron microscope analysis. Band gap energy of synthesised nanocrystalline ZnO was calculated using diffuse reflectance spectroscopy (DRS). Different experimental parameters such as effects of pH, dye concentrations and mass of catalyst were standardised in order to achieve complete degradation of the dye molecules under solar light irradiation. The kinetics of oxidation of OG was also studied. The complete degradation of OG was evident after 90 min of irradiation at an initial pH of 6.86. The degradation of OG was confirmed by UV-Visible spectrophotometer, high-pressure liquid chromatography, ESI-Mass and chemical oxygen demand analyses. The adsorption of dye onto catalytic surface was analysed employing model equations such as Langmuir and Freundlich isotherms, and it was found that the Langmuir isotherm model best fitted the adsorption data. The solar photodegradation of OG followed pseudo-first-order kinetics. HPLC and ESI-Mass analyses of the degraded samples suggested that the dye molecules were readily degraded under solar irradiation with nanocrystalline ZnO.

Comparison of quartz crystallographic preferred orientations identified with optical fabric analysis, electron backscatter and neutron diffraction techniques.

PubMed

Hunter, N J R; Wilson, C J L; Luzin, V

2017-02-01

Three techniques are used to measure crystallographic preferred orientations (CPO) in a naturally deformed quartz mylonite: transmitted light cross-polarized microscopy using an automated fabric analyser, electron backscatter diffraction (EBSD) and neutron diffraction. Pole figure densities attributable to crystal-plastic deformation are variably recognizable across the techniques, particularly between fabric analyser and diffraction instruments. Although fabric analyser techniques offer rapid acquisition with minimal sample preparation, difficulties may exist when gathering orientation data parallel with the incident beam. Overall, we have found that EBSD and fabric analyser techniques are best suited for studying CPO distributions at the grain scale, where individual orientations can be linked to their source grain or nearest neighbours. Neutron diffraction serves as the best qualitative and quantitative means of estimating the bulk CPO, due to its three-dimensional data acquisition, greater sample area coverage, and larger sample size. However, a number of sampling methods can be applied to FA and EBSD data to make similar approximations. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

The molecular structure of 4-methylpyridine-N-oxide: Gas-phase electron diffraction and quantum chemical calculations

NASA Astrophysics Data System (ADS)

Belova, Natalya V.; Girichev, Georgiy V.; Kotova, Vitaliya E.; Korolkova, Kseniya A.; Trang, Nguyen Hoang

2018-03-01

The molecular structure of 4-methylpiridine-N-oxide, 4-MePyO, has been studied by gas-phase electron diffraction monitored by mass spectrometry (GED/MS) and quantum chemical (DFT) calculations. Both, quantum chemistry and GED analyses resulted in CS molecular symmetry with the planar pyridine ring. Obtained molecular parameters confirm the hyperconjugation in the pyridine ring and the sp2 hybridization concept of the nitrogen and carbon atoms in the ring. The experimental geometric parameters are in a good agreement with the parameters for non-substituted N-oxide and reproduced very closely by DFT calculations. The presence of the electron-donating CH3 substituent in 4-MePyO leads to a decrease of the ipso-angle and to an increase of r(N→O) in comparison with the non-substituted PyO. Electron density distribution analysis has been performed in terms of natural bond orbitals (NBO) scheme. The nature of the semipolar N→O bond is discussed.

Physicochemical behavior of several kinds of paper under gamma irradiation

NASA Astrophysics Data System (ADS)

Jiménez-Reyes, Melania; Tenorio, Dolores; Rojas-Robles, Mariela; García-Rosales, Genoveva

2018-07-01

Several kinds of paper (Bond, Amate, Rice, Press, and Whatman#1) were studied in their original condition and were then exposed to gamma radiation between 3 and 15 kGy (0.9 kGy/h) with intervals of 3 kGy. The length and width of fibers (SEM) as well as pH were measured, and the chemical composition was determined by EDS. Pyrolysis characteristics (TGA and DTC), transmittance spectra by IR and X-ray diffraction patterns were studied as well. Whatman#1 contains only cellulose; whereas Bond, Press and Rice papers also contain calcite and Amate whewellite. All X-ray diffraction patterns showed Type I semicrystalline cellulose, but a slight presence of Type II was noted in the artisan papers (Amate and Rice). These results were confirmed by IR spectra and thermogravimetric analyses. Due to gamma irradiation no acidification nor change of fiber sizes or alteration of other studied parameters were observed. Therefore, these conditions may be recommended for the treatment of some deteriorated documents.

Effect of radiation induced crosslinking and degradation of ETFE films

NASA Astrophysics Data System (ADS)

Zen, H. A.; Ribeiro, G.; Geraldes, A. N.; Souza, C. P.; Parra, D. F.; Lugão, A. B.

2013-03-01

In this study the ETFE film with 125 μm of thickness was placed inside a nylon bag and filled with either acetylene, nitrogen or oxygen. Following the procedure, the samples were irradiated at 5, 10 and 20 kGy. The physical and chemical properties of the modified and pristine films were evaluated by rheological and thermal analyses (TG and DSC), X-ray diffraction (XRD) and infrared spectroscopy (IR-ATR). In rheological analysis the storage modulus (G') indicates opposite profiles when the atmospheres (acetylene and oxygen) are evaluated according to the absorbed dose. For the samples submitted to radiation under oxygen atmosphere it is possible to observe the degradation process with the low levels of the storage modulus. The changes in the degree of crystallinity were verified in all modified samples when compared to the pristine polymer and this behavior was confirmed by DSC analysis. A decrease in the intensity of crystalline peak by X-ray diffraction was observed.

Synthesis, structural, spectroscopic and optical studies of charge transfer complex salts.

PubMed

Manikandan, Maruthappan; Mahalingam, Thaiyan; Hayakawa, Yasuhiro; Ravi, Ganesan

2013-01-15

New charge transfer molecular complex adducts of picric acid (C6H3N3O7) with triethylamine (C6H15N) and dimethylformamide (HCON(CH3)2) were synthesized successfully for the first time. Chemical composition and stoichiometry of the synthesized complex salts were verified by CHN elemental analysis. Solubility of the complex salts have been determined by gravimetric method and single crystals of two new salts were grown by low temperature solution growth technique. Crystal system, crystalline nature and cell parameters of the grown crystals were determined by single crystal X-ray diffraction (SXRD) and powder X-ray diffraction (PXRD) analyses. The formations of the charge-transfer complex, functional groups and the modes of vibrations have been confirmed by Fourier transform infrared (FTIR) spectroscopy. In order to know the linear and nonlinear optical suitability for device fabrication, UV-Vis (UV) spectral analysis and relative second harmonic generation (SHG) efficiency test were performed for the grown crystals. Copyright © 2012 Elsevier B.V. All rights reserved.

Search for dilute excited states in 16O

NASA Astrophysics Data System (ADS)

Ogloblin, A. A.; Danilov, A. N.; Demyanova, A. S.; Goncharov, S. A.; Belyaeva, T. L.

2016-11-01

The root mean square radii of 16O in the short-lived 0+ excited states were experimentally deduced for the first time from the analyses of α +16O diffraction scattering. Differential cross sections of the elastic and inelastic α +16O and 16O+16O scattering in the incident energy range from a few MeV/nucleon up to 100 MeV/nucleon were analyzed by the modified diffraction model. No significant radius enhancement in any state in comparison with the ground state was observed. This concerns, in particular, the 15.1-MeV 06+ state of 16O, located in the vicinity of the four-α -particle complete dissociation threshold, for which we did not confirm the "gigantic" size predicted by the α -particle condensation model. This result does not support the idea that 16O in the 06+ state has a dilute structure and can be considered as an analog of the famous 7.65-MeV 02+ Hoyle state of 12C.

Biosynthesis of silver nanoparticles using aqueous leaf extract of Thevetia peruviana Juss and its antimicrobial activities

NASA Astrophysics Data System (ADS)

Oluwaniyi, Omolara O.; Adegoke, Haleemat I.; Adesuji, Elijah T.; Alabi, Aderemi B.; Bodede, Sunday O.; Labulo, Ayomide H.; Oseghale, Charles O.

2016-08-01

Biosynthesizing of silver nanoparticles using microorganisms or various plant parts have proven more environmental friendly, cost-effective, energy saving and reproducible when compared to chemical and physical methods. This investigation demonstrated the plant-mediated synthesis of silver nanoparticles using the aqueous leaf extract of Thevetia peruviana. UV-Visible spectrophotometer was used to measure the surface plasmon resonance of the nanoparticles at 460 nm. Fourier Transform Infrared showed that the glycosidic -OH and carbonyl functional group present in extract were responsible for the reduction and stabilization of the silver nanoparticles. X ray diffraction, Scanning Electron Microscopy, Transmission Electron Microscopy and Selected Area Electron Diffraction analyses were used to confirm the nature, morphology and shape of the nanoparticles. The silver nanoparticles are spherical in shape with average size of 18.1 nm. The synthesized silver nanoparticles showed activity against fungal pathogens and bacteria. The zone of inhibition observed in the antimicrobial study ranged between 10 and 20 mm.

Synthesis, structural, spectroscopic and optical studies of charge transfer complex salts

NASA Astrophysics Data System (ADS)

Manikandan, Maruthappan; Mahalingam, Thaiyan; Hayakawa, Yasuhiro; Ravi, Ganesan

2013-01-01

New charge transfer molecular complex adducts of picric acid (C6H3N3O7) with triethylamine (C6H15N) and dimethylformamide (HCON(CH3)2) were synthesized successfully for the first time. Chemical composition and stoichiometry of the synthesized complex salts were verified by CHN elemental analysis. Solubility of the complex salts have been determined by gravimetric method and single crystals of two new salts were grown by low temperature solution growth technique. Crystal system, crystalline nature and cell parameters of the grown crystals were determined by single crystal X-ray diffraction (SXRD) and powder X-ray diffraction (PXRD) analyses. The formations of the charge-transfer complex, functional groups and the modes of vibrations have been confirmed by Fourier transform infrared (FTIR) spectroscopy. In order to know the linear and nonlinear optical suitability for device fabrication, UV-Vis (UV) spectral analysis and relative second harmonic generation (SHG) efficiency test were performed for the grown crystals.

Synthesis and spectral studies on Cd(II) dithiocarbamate complexes and their use as precursors for CdS nanoparticles

NASA Astrophysics Data System (ADS)

Sathiyaraj, Ethiraj; Padmavathy, Krishnaraj; Kumar, Chandran Udhaya; Krishnan, Kannan Gokula; Ramalingan, Chennan

2017-11-01

Bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (1) and (2,2‧-bipyridine) bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (2) have been synthesized and characterized by FT-IR, 1HNMR and 13C NMR analyses. For the complex 2, single crystal X-ray diffraction analysis and computational studies (optimized geometry, HOMO-LUMO and MEP) have been executed employing DFT/B3LYP method with LANL 2DZ basic set. The optimized bond lengths and bond angles agree well with the experimental results. The complexes 1 and 2 have been used as single source precursors for the synthesis of ethyleneglycol capped CdS1 and CdS2 nanoparticles, respectively. CdS1 and CdS2 nanoparticles have been synthesized by solvothermal method. PXRD, SEM, Elemental colour mapping, EDAX, TEM and UV-Vis spectroscopy have been used to characterize the as-prepared CdS nanoparticles. The X-ray diffraction pattern confirms both their hexagonal structures.

Synthesis, characterization, temperature dependent electrical and magnetic properties of Ca3Co4O9 by a starch assisted sol-gel combustion method

NASA Astrophysics Data System (ADS)

Agilandeswari, K.; Ruban Kumar, A.

2014-09-01

In this present work we discussed the synthesis of pure Ca3Co4O9 ceramic powder by a starch assisted sol-gel combustion method. The products were characterized by powder X-ray diffraction (XRD), thermogravimetric and differential thermal analyses (TGA-DTA), Fourier transformation infrared spectroscopy (FTIR), scanning electron microscope (SEM) and UV-visible diffuse reflectance spectroscopy (DRS). X-ray diffraction pattern confirmed the formation of single phase Ca3Co4O9 at a sintering temperature of 1073 K, and it is also confirmed in the thermal analysis. SEM images indicate the presence of diffused microporous sphere like morphology and the grain sizes are in the range of 150-300 nm. Optical properties of Ca3Co4O9 ceramic show a band gap at an energy level of 2.10 eV. A maximum electrical resistivity of 0.002 mΩ cm was exhibited by Ca3Co4O9 that was decreased to 0.0012 mΩ cm, when the temperature increased from 300 K to 473 K. Dielectric studies were conducted at various temperatures from room temperature to 673 K and the results indicate that the space charge polarization contributes to the conduction mechanism. It also shows that the dielectric relaxation with activation energy is 0.96 eV. The magnetic properties as a function of temperature represent the ferri-paramagnetic phase transition at above 50 K. M-H curve shows the hysteresis loop with saturation magnetization (Ms) and confirms the presence of soft magnetic materials.

Absolute configuration of a chiral CHD group via neutron diffraction: confirmation of the absolute stereochemistry of the enzymatic formation of malic acid

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

Bau, R.; Brewer, I.; Chiang, M.Y.

Neutron diffraction has been used to monitor the absolute stereochemistry of an enzymatic reaction. (-)(2S)malic-3-d acid was prepared by the action of fumarase on fumaric acid in D/sub 2/O. After a large number of cations were screened, it was found that (+)(R)..cap alpha..-phenylethylamine forms the large crystals necessary for a neutron diffraction analysis. The subsequent structure determination showed that (+)(R)..cap alpha..-phenylethylammonium (-)(2S)malate-3-d has an absolute configuration of R at the CHD site. This result confirms the absolute stereochemistry of fumarate-to-malate transformation as catalyzed by the enzyme fumarase.

Electrochemical alloying of immiscible Ag and Co for their structural and magnetic analyses

NASA Astrophysics Data System (ADS)

Santhi, Kalavathy; Kumarsan, Dhanapal; Vengidusamy, Naryanan; Arumainathan, Stephen

2017-07-01

Electrochemical alloying of immiscible Ag and Co was carried out at different current densities from electrolytes of two different concentrations, after optimizing the electrolytic bath and operating conditions. The samples obtained were characterized using X-ray diffraction to confirm the simultaneous deposition of Ag and Co and to determine their crystallographic structure. The atomic percentage of Ag and Co contents in the granular alloy was determined by ICP-OES analysis. The XPS spectra were observed to confirm the presence of Ag and Co in the metallic form in the granular alloy samples. The micrographs observed using scanning and transmission electron microscopes threw light on the surface morphology and the size of the particles. The magnetic nature of the samples was analyzed at room temperature by a vibration sample magnetometer. Their magnetic phase transition while heating was also studied to provide further evidence for the magnetic behaviour and the structure of the deposits.

New polyurethane nanocomposites based on soya oil.

PubMed

Mohammed, Issam Ahmed; Abd Khadir, Nurul Khizrien; Jaffar Al-Mulla, Emad Abbas

2014-01-01

New polyurethane (PU) nanocomposites were prepared from a dispersion of 0 - 5% montmorillonite (MMT) clay with isocyanate and soya oil polyol that was synthesized via transesterification of triglycerides to reduce petroleum dependence. FT-IR spectra indicate the presence of hydrogen bonding between nanoclay and the polymer matrix, whereas the exfoliated structure of clay layers was confirmed by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Optical microscopy, mechanical and thermal analyses were done to investigate significant improvement of the nanocomposites. The results showed PU-3% nanoclay (NC) showed optimum results in mechanical properties such as tensile and flexural strength but the lowest in impact strength.

Novel synthesis strategy for composite hydrogel of collagen/hydroxyapatite-microsphere originating from conversion of CaCO3 templates.

PubMed

Wei, Qingrong; Lu, Jian; Wang, Qiaoying; Fan, Hongsong; Zhang, Xingdong

2015-03-20

Inspired by coralline-derived hydroxyapatite, we designed a methodological route to synthesize carbonated-hydroxyapatite microspheres from the conversion of CaCO3 spherulite templates within a collagen matrix under mild conditions and thus constructed the composite hydrogel of collagen/hydroxyapatite-microspheres. Fourier transform infrared spectroscopy (FTIR) and x-ray diffraction (XRD) were employed to confirm the successful generation of the carbonated hydroxyapatite phase originating from CaCO3, and the ratios of calcium to phosphate were tracked over time. Variations in the weight portion of the components in the hybrid gels before and after the phase transformation of the CaCO3 templates were identified via thermogravimetric analysis (TGA). Scanning electron microscopy (SEM) shows these composite hydrogels have a unique multiscale microstructure consisting of a collagen nanofibril network and hydroxyapatite microspheres. The relationship between the hydroxyapatite nanocrystals and the collagen fibrils was revealed by transmission electron microscopy (TEM) in detail, and the selected area electron diffraction (SAED) pattern further confirmed the results of the XRD analyses which show the typical low crystallinity of the generated hydroxyapatite. This smart synthesis strategy achieved the simultaneous construction of microscale hydroxyapatite particles and collagen fibrillar hydrogel, and appears to provide a novel route to explore an advanced functional hydrogel materials with promising potentials for applications in bone tissue engineering and reconstruction medicine.

Synthesis and characterization of Mg-Al-layered double hydroxides intercalated with cubane-1,4-dicarboxylate anions.

PubMed

Rezvani, Zolfaghar; Arjomandi Rad, Farzad; Khodam, Fatemeh

2015-01-21

In the present work, Mg2Al-layered double hydroxide (LDH) intercalated with cubane-1,4-dicarboxylate anions was prepared from the reaction of solutions of Mg(ii) and Al(iii) nitrate salts with an alkaline solution of cubane-1,4-dicarboxylic acid by using the coprecipitation method. The successful preparation of a nanohybrid of cubane-1,4-dicarboxylate(cubane-dc) anions with LDH was confirmed by powder X-ray diffraction, FTIR spectroscopy and thermal gravimetric analysis (TGA). The increase in the basal spacing of LDHs from 8.67 Å to 13.40 Å shows that cubane-dc anions were successfully incorporated into the interlayer space. Thermogravimetric analyses confirm that the thermal stability of the intercalated cubane-dc anions is greater than that of the pure form before intercalation because of host-guest interactions involving hydrogen bonds. The interlayer structure, hydrogen bonding, and subsequent distension of LDH compounds containing cubane-dc anions were shown by molecular simulation. The RDF (radial distribution function), mean square displacement (MSD), and self-diffusion coefficient were calculated using the trajectory files on the basis of molecular dynamics (MD) simulations, and the results indicated that the cubane-dc anions were more stable when intercalated into the LDH layers. A good agreement was obtained between calculated and measured X-ray diffraction patterns and between experimental and calculated basal spacings.

TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Shirahama, Keiya; Torizuka, Yasufumi; Manoda, Masahiro; Nakasako, Masayoshi; Yamamoto, Masaki

2016-05-01

Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speed higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens.

New test of the dynamic theory of neutron diffraction by a moving grating

NASA Astrophysics Data System (ADS)

Zakharov, Maxim; Frank, Alexander; Kulin, German; Goryunov, Semyon

2018-04-01

Recently, multiwave dynamical theory of neutron diffraction by a moving grating was developed. The theory predicts that at a certain height of the grating profile a significant suppression of the zero-order diffraction may occur. The experiment to confirm predictions of this theory was performed. The resulting diffracted UCNs spectra were measured using time-of-flight Fourier diffractometer. The experimental data were compared with the results of numerical simulation and were found in a good agreement with theoretical predictions.

Electron microscopy analyses and electrical properties of the layered Bi{sub 2}WO{sub 6} phase

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

Taoufyq, A.; Laboratoire Matériaux et Environnement LME, Faculté des Sciences, Université Ibn Zohr, BP 8106, Cité Dakhla, Agadir, Maroc; Département d‘Études des Réacteurs, Laboratoire Dosimétrie Capteurs Instrumentation, CEA Cadarache

2013-07-15

The bismuth tungstate Bi{sub 2}WO{sub 6} was synthesized using a classical coprecipitation method followed by a calcination process at different temperatures. The samples were characterized by X-ray diffraction, simultaneous thermogravimetry and differential thermal analysis (TGA/DTA), scanning and transmission electron microscopy (SEM, TEM) analyses. The Rietveld analysis and electron diffraction clearly confirmed the Pca2{sub 1} non centrosymmetric space group previously proposed for this phase. The layers Bi{sub 2}O{sub 2}{sup 2+} and WO{sub 4}{sup 2−} have been directly evidenced from the HRTEM images. The electrical properties of Bi{sub 2}WO{sub 6} compacted pellets systems were determined from electrical impedance spectrometry (EIS) and directmore » current (DC) analyses, under air and argon, between 350 and 700 °C. The direct current analyses showed that the conduction observed from EIS analyses was mainly ionic in this temperature range, with a small electronic contribution. Electrical change above the transition temperature of 660 °C is observed under air and argon atmospheres. The strong conductivity increase observed under argon is interpreted in terms of formation of additional oxygen vacancies coupled with electron conduction. - Graphical abstract: High resolution transmission electron microscopy: inverse fast Fourier transform giving the layered structure of the Bi{sub 2}WO{sub 6} phase, with a representation of the cell dimensions (b and c vectors). The Bi{sub 2}O{sub 2}{sup 2+} and WO{sub 4}{sup 2−} sandwiches are visible in the IFFT image. - Highlights: • Using transmission electron microscopy, we visualize the layered structure of Bi{sub 2}WO{sub 6}. • Electrical analyses under argon gas show some increase in conductivity. • The phase transition at 660 °C is evidenced from electrical modification.« less

Diffraction of three-colour radiation on an acoustic wave

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

Kotov, V M

We study acousto-optic Bragg diffraction of three-colour radiation having wavelengths of 488, 514 and 633 nm on a single acoustic wave propagating in a TeO{sub 2} crystal. A technique is developed that allows one to find diffraction regimes with a proportional change in the intensity of all radiations by varying the acoustic power. According to the technique, radiation with a maximum wavelength has to be in strict Bragg synchronism with the acoustic wave, while other radiations diffract during the synchronism detuning. The results obtained using this technique are experimentally confirmed. (diffraction of light)

Synthesis and characterization of Chitosan-CuO-MgO polymer nanocomposites

NASA Astrophysics Data System (ADS)

Praffulla, S. R.; Bubbly, S. G.

2018-05-01

In the present work, we have synthesized Chitosan-CuO-MgO nanocomposites by incorporating CuO and MgO nanoparticles in chitosan matrix. Copper oxide and magnesium oxide nanoparticles synthesized by precipitation method were characterized by X-ray diffraction and the diffraction patterns confirmed the monoclinic and cubic crystalline structures of CuO and MgO nanoparticles respectively. Chitosan-CuO-MgO composite films were prepared using solution- cast method with different concentrations of CuO and MgO nanoparticles (15 - 50 wt % with respect to chitosan) and characterized by XRD, FTIR and UV-Vis spectroscopy. The X-ray diffraction pattern shows that the crystallinity of the chitosan composite increases with increase in nanoparticle concentration. FTIR spectra confirm the chemical interaction between chitosan and metal oxide nanoparticles (CuO and MgO). UV absorbance of chitosan nanocomposites were up to 17% better than pure chitosan, thus confirming its UV shielding properties. The mechanical and electrical properties of the prepared composites are in progress.

Diffraction effect of the injected beam in axisymmetrical structural CO2 laser

NASA Astrophysics Data System (ADS)

Xu, Yonggen; Wang, Shijian; Fan, Qunchao

2012-07-01

Diffraction effect of the injected beam in axisymmetrical structural CO2 laser is studied based on the injection-locking principle. The light intensity of the injected beam at the plane where the holophotes lie is derived according to the Huygens-Fresnel diffraction integral equation. And then the main parameters which influence the diffraction light intensity are given. The calculated results indicate that the first-order diffraction signal will play an important role in the phase-locking when the zero-order diffraction cannot reach the folded cavities. The numerical examples are given to confirm the correctness of the results, and the comparisons between the theoretical and the experimental results are illustrated.

Radiation damage and annealing in plutonium tetrafluoride

NASA Astrophysics Data System (ADS)

McCoy, Kaylyn; Casella, Amanda; Sinkov, Sergey; Sweet, Lucas; McNamara, Bruce; Delegard, Calvin; Jevremovic, Tatjana

2017-12-01

A sample of plutonium tetrafluoride that was separated prior to 1966 at the Hanford Site in Washington State was analyzed at the Pacific Northwest National Laboratory (PNNL) in 2015 and 2016. The plutonium tetrafluoride, as received, was an unusual color and considering the age of the plutonium, there were questions about the condition of the material. These questions had to be answered in order to determine the suitability of the material for future use or long-term storage. Therefore, thermogravimetric/differential thermal analysis and X-ray diffraction evaluations were conducted to determine the plutonium's crystal structure, oxide content, and moisture content; these analyses reported that the plutonium was predominately amorphous and tetrafluoride, with an oxide content near ten percent. Freshly fluorinated plutonium tetrafluoride is known to be monoclinic. During the initial thermogravimetric/differential thermal analyses, it was discovered that an exothermic event occurred within the material near 414 °C. X-ray diffraction analyses were conducted on the annealed tetrafluoride. The X-ray diffraction analyses indicated that some degree of recrystallization occurred in conjunction with the 414 °C event. The following commentary describes the series of thermogravimetric/differential thermal and X-ray diffraction analyses that were conducted as part of this investigation at PNNL.

TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA

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

Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka

Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speedmore » higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens.« less

Optical Tweezers for Sample Fixing in Micro-Diffraction Experiments

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

Amenitsch, H.; Rappolt, M.; Sartori, B.

2007-01-19

In order to manipulate, characterize and measure the micro-diffraction of individual structural elements down to single phospholipid liposomes we have been using optical tweezers (OT) combined with an imaging microscope. We were able to install the OT system at the microfocus beamline ID13 at the ESRF and trap clusters of about 50 multi-lamellar liposomes (< 10 {mu}m large cluster). Further we have performed a scanning diffraction experiment with a 1 micrometer beam to demonstrate the fixing capabilities and to confirm the size of the liposome cluster by X-ray diffraction.

Synthesis, growth, structural and optical studies of a novel organic Piperazine (bis) p-toluenesulfonate single crystal.

PubMed

Rekha, P; Peramaiyan, G; NizamMohideen, M; Kumar, R Mohan; Kanagadurai, R

2015-03-15

A novel organic single crystal of Piperazinium (bis) p-toluenesulfonate (PPTS) was grown by a slow evaporation solution growth technique. The structure of the grown crystal was determined using single crystal X-ray diffraction analysis. The PPTS crystal belongs to the triclinic crystal system with space group of P1¯. The presence of functional groups was confirmed by FTIR spectral analysis. The optical transmittance range and cut-off wavelength were identified by UV-vis-NIR spectral studies. The luminescent properties of PPTS crystal were investigated. The thermal behavior of PPTS crystal was studied by TG-DT analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis, structural, thermal and optical studies of 1-ethyl-2,6-dimethyl-4-hydroxy pyridinium halides.

PubMed

Dhanuskodi, S; Manivannan, S; Kirschbaum, K

2006-05-15

1-Ethyl-2,6-dimethyl-4-hydroxy pyridinium chloride dihydrate and bromide dihydrate salts have been synthesized and their single crystals were grown by the slow evaporation of aqueous solution at 30 degrees C. The grown crystals were characterized by elemental analysis, FT-NMR and FT-IR techniques to confirm the formation of the expected compound. Optical transmittance window in aqueous solution was found to be 275-1100 nm by UV-vis-NIR technique. Thermogravimetric and differential thermal analyses reveal thermal stability and the presence of two water molecules in the crystal lattices. The crystal structure of chloride salt was also determined by X-ray diffraction method.

Coal and cremation at the Tschudi burn, Chan Chan, Northern Peru

USGS Publications Warehouse

Brooks, W.E.; Galvez, Mora C.; Jackson, J.C.; McGeehin, J.P.; Hood, D.G.

2008-01-01

Analyses of a 20-30 cm thick, completely combusted ash at the 25 ?? 70 m Tschudi burn at Chan Chan, northern Peru??, contain 52-55 wt% SiO2, 180-210 ppm zirconium and are consistent with coal ash. Soil geochemistry across the burn showed elevated calcium and phosphorus content, possible evidence for reported human cremation. A calcined, 5 g, 4.5 cm skull fragment recovered from the burn was confirmed as human by protein radioimmunoassay (pRIA). X-ray diffraction showed that the bone had been heated to 520??C. The burn took place c. ad 1312-1438 based on interpretation of a 14C date on carbonized plant tinder. ?? 2008 University of Oxford.

Synthesis and reactions of C-phosphanylated thiazol-2-thiones.

PubMed

Begum, I; Schnakenburg, G; Streubel, R

2016-02-21

The facile regioselective synthesis of the P(iii) substituted thiazol-2-thione 2 is presented. Reaction of 2 with hydrogenperoxide-urea, elemental sulfur and selenium resulted in P(v) chalcogenide thiazol-2-thiones 3-5. All compounds were characterized using (31)P, (1)H, (13)C NMR, IR and elemental analyses and, additionally, by the single-crystal X-ray diffraction technique. Oxidative desulfurization of the 5-phosphinoylated thiazol-2-thione 3 using hydrogenperoxide led to the first C-phosphanoyl substituted thiazolium salt (6). Deprotonation of 6 and in situ reaction with the cyclooctadiene rhodium(i) chloride dimer yielded thiazol-2-ylidene rhodium(i) complex 7 which was confirmed by NMR spectroscopy and ESI-MS spectrometry.

Synthesis and electrochemical property of few-layer molybdenum disulfide nanosheets

NASA Astrophysics Data System (ADS)

Fu, Yanjue; Wang, Chunrui; Wang, Linlin; Peng, Xia; Wu, Binhe; Sun, Xingqu; Chen, Xiaoshuang

2016-12-01

Large-scale few-layer MoS2 nanosheets have been fabricated via a simple hydrothermal route using molybdenum powder as precursors. The as-prepared MoS2 samples were characterized by X-ray powder diffraction (XRD) analysis, transmission electron microscopy (TEM), and Raman and photoluminescence (PL) spectral analyses at room temperature. The results confirm that the as-prepared MoS2 displays a sheet-like morphology with a thickness of few (bi- to tri-) layers. Electrochemical measurements showed that the as-prepared few-layer MoS2 exhibited the highest reversible capacity of 1127 mAh g-1 and a stable reversible capacity of 1057 mAh g-1 after 30 cycles.

Cl⋯N weak interactions. Conformational analysis of imidazol-2-ylum heterocycles bearing N-β-chloroethyl and N-vinyl pendant groups

NASA Astrophysics Data System (ADS)

Rodríguez-López, Germán; Montes-Tolentino, Pedro; Sánchez-Ruiz, Sonia; Villaseñor-Granados, Tayde Osvaldo; Flores-Parra, Angelina

2017-11-01

Enantiomerically pure and racemic mixtures of β-chloroethylamines hydrochlorides with one and two stereogenic centres were used to synthesise 1,4-dialkyl-1,3-diimines, which in turn gave place to a series of imidazolium chlorides and tetraphenylborates bearing pendant N-β-chloroethyl substituents (sbnd CHEt-CH2Cl; sbnd CHMe-CHPhCl). Stereoselective dehydrochlorination of imidazolium compounds afforded in good yield the corresponding heterocycles bearing N-vinyl groups (-CEt=CH2; -CMe=CHPh). The volume of the N-substituents provides a steric screening of the cationic ring. The structure of the new compounds was determined by IR, mass spectra, NMR and X-ray diffraction analyses as well as DFT calculations of the optimized geometries. Uncommon stabilising intramolecular Cl⋯N weak interactions are described, together with H⋯Cl and H···π hydrogen bonds. The existence of the non-covalent weak intramolecular bonds was deduced from the X-ray diffraction analysis and confirmed by calculations of the electrostatic potential, electronic density distributions and the maps of the Laplacian functions of the electronic density.

Hydrothermal synthesis, crystal structures, and enantioselective adsorption property of bis(L-histidinato)nickel(II) monohydrate

NASA Astrophysics Data System (ADS)

Ramos, Christian Paul L.; Conato, Marlon T.

2018-05-01

Despite the numerous researches in metal-organic frameworks (MOFs), there are only few reports on biologically important amino acids, histidine in particular, on its use as bridging ligand in the construction of open-framework architectures. In this work, hydrothermal synthesis was used to prepare a compound based on Ni2+ and histidine. The coordination assembly of imidazole side chain of histidine with divalent nickel ions in aqueous condition yielded purple prismatic solids. Single crystal X-ray diffraction (XRD) analysis of the product revealed structure for Ni(C6H8N3O2)2 • H2O that has a monoclinic (C2) structure with lattice parameters, a = 29.41, b = 8.27, c = 6.31 Å, β = 90.01 ˚. Circular dichroism - optical rotatory dispersion (CD-ORD), Powder X-ray diffraction (PXRD) and Fourier transform - infrared spectroscopy (FT-IR) analyses are conducted to further characterize the crystals. Enantioselective adsorption analysis using racemic mixture of 2-butanol confirmed bis(L-histidinato)nickel(II) monohydrate MOF crystal's enantioselective property preferentially favoring the adsorption of (S)-2-butanol isomer.

Green synthesis of gold nanoparticles using chlorogenic acid and their enhanced performance for inflammation.

PubMed

Hwang, Su Jung; Jun, Sang Hui; Park, Yohan; Cha, Song-Hyun; Yoon, Minho; Cho, Seonho; Lee, Hyo-Jong; Park, Youmie

2015-10-01

Here we developed a novel green synthesis method for gold nanoparticles (CGA-AuNPs) using chlorogenic acid (CGA) as reductants without the use of other chemicals and validated the anti-inflammatory efficacy of CGA-AuNPs in vitro and in vivo. The resulting CGA-AuNPs appeared predominantly spherical in shape with an average diameter of 22.25±4.78nm. The crystalline nature of the CGA-AuNPs was confirmed by high-resolution X-ray diffraction and by selected-area electron diffraction analyses. High-resolution liquid chromatography/electrospray ionization mass spectrometry revealed that the caffeic acid moiety of CGA forms quinone structure through a two-electron oxidation causing the reduction of Au(3+) to Au(0). When compared to CGA, CGA-AuNPs exhibited enhanced anti-inflammatory effects on NF-κB-mediated inflammatory network, as well as cell adhesion. Collectively, green synthesis of CGA-AuNPs using bioactive reductants and mechanistic studies based on mass spectrometry may open up new directions in nanomedicine and CGA-AuNPs can be an anti-inflammatory nanomedicine for future applications. Gold nanoparticles (Au NPs) have been shown to be very useful in many applications due to their easy functionalization capability. In this article, the authors demonstrated a novel method for the synthesis of gold nanoparticles using chlorogenic acid (CGA) as reductants. In-vitro experiments also confirmed biological activity of the resultant gold nanoparticles. Further in-vivo studies are awaited. Copyright © 2015 Elsevier Inc. All rights reserved.

Radiation damage and annealing in plutonium tetrafluoride

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

McCoy, Kaylyn; Casella, Amanda; Sinkov, Sergey

Plutonium tetrafluoride that was separated prior to 1966 at the Hanford Site in Washington State was analyzed at the Pacific Northwest National Laboratory (PNNL) in 2015 and 2016. The plutonium tetrafluoride, as received, was an off-normal color and considering the age of the plutonium, there were questions about the condition of the material. These questions had to be answered in order to determine the suitability of the material for future use or long-term storage. Therefore, Thermogravimetric/Differential Thermal Analysis and X-ray Diffraction evaluations were conducted to determine the plutonium’s crystal structure, oxide content, and moisture content; these analyses reported that themore » plutonium was predominately amorphous and tetrafluoride, with an oxide content near ten percent. Freshly fluorinated plutonium tetrafluoride is known to be monoclinic. During the initial Thermogravimetric/Differential Thermal analyses, it was discovered that an exothermic event occurred within the material near 414°C. X-ray Diffraction analyses were conducted on the annealed tetrafluoride. The X-ray Diffraction analyses indicated that some degree of recrystallization occurred in conjunction with the 414°C event. The following commentary describes the series of Thermogravimetric/Differential Thermal and X-ray Diffraction analyses that were conducted as part of this investigation at PNNL, in collaboration with the University of Utah Nuclear Engineering Program.« less

Optical, mechanical and thermal behaviors of Nitrilotriacetic acid single crystal

NASA Astrophysics Data System (ADS)

Deepa, B.; Philominathan, P.

2017-11-01

An organic nonlinear single crystal of Nitrilotriacetic acid (NTAA) was grown for the first time by employing a simple slow evaporation technique. Single crystal X-ray diffraction (XRD) analysis reveals that the grown crystal belongs to the monoclinic system with noncentrosymmetric space group CC. Fourier transform infrared (FTIR) spectral study ascertains the presence of functional groups in NTAA. The molecular structure of the grown crystal was confirmed by Nuclear Magnetic Resonance (NMR) spectral analysis. The optical parameters such as transmittance, absorption coefficient and band gap were calculated from UV-Visible and fluorescence studies. Dielectric measurements were carried out for different frequency and temperature. The mechanical strength of the grown crystal was measured using Vickers microhardness test. The high thermal stability and the melting point of the grown crystal were also estimated using thermogravimetric (TGA) and differential thermal analyses (DTA). The confirmation of the grown crystals belonging to nonlinear optical crystals was performed by Kurtz-Perry technique and found as suitable candidate for optoelectronics applications.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Room Temperature Elastic Moduli and Vickers Hardness of Hot-Pressed LLZO Cubic Garnet

DTIC Science & Technology

2012-01-01

polishing compounds, Leco, St. Joseph, MI). X - ray diffraction and scanning electron microscopy (SEM) The microstructure of the hot-pressed specimens...was examined on uncoated fracture surfaces by SEM with an accelerating voltage of 1 and 3 kV. Phase purity was evaluated from X - ray diffraction data...the micro- structure appeared to be homogenous for the two hot- pressed LLZO specimens included in this study (Fig. 1). X - ray diffraction confirmed that

Resolution enhancement in coherent x-ray diffraction imaging by overcoming instrumental noise.

PubMed

Kim, Chan; Kim, Yoonhee; Song, Changyong; Kim, Sang Soo; Kim, Sunam; Kang, Hyon Chol; Hwu, Yeukuang; Tsuei, Ku-Ding; Liang, Keng San; Noh, Do Young

2014-11-17

We report that reference objects, strong scatterers neighboring weak phase objects, enhance the phase retrieval and spatial resolution in coherent x-ray diffraction imaging (CDI). A CDI experiment with Au nano-particles exhibited that the reference objects amplified the signal-to-noise ratio in the diffraction intensity at large diffraction angles, which significantly enhanced the image resolution. The interference between the diffracted x-ray from reference objects and a specimen also improved the retrieval of the phase of the diffraction signal. The enhancement was applied to image NiO nano-particles and a mitochondrion and confirmed in a simulation with a bacteria phantom. We expect that the proposed method will be of great help in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

A portable X-ray diffraction apparatus for in situ analyses of masters' paintings

NASA Astrophysics Data System (ADS)

Eveno, Myriam; Duran, Adrian; Castaing, Jacques

2010-09-01

It is rare that the analyses of materials in paintings can be carried out by taking micro-samples. Valuable works of art are best studied in situ by non-invasive techniques. For that purpose, a portable X-ray diffraction and fluorescence apparatus has been designed and constructed at the C2RMF. This apparatus has been used for paintings of Rembrandt, Leonardo da Vinci, Van Gogh, Mantegna, etc. Results are given to illustrate the performance of X-ray diffraction, especially when X-ray fluorescence does not bring sufficient information to conclude.

Lattice-Preferred Orientation in Deformed Novaculite - Comparison of in-situ Results Using BEARTEX and Post-Mortem EBSD Analyses

NASA Astrophysics Data System (ADS)

Willenweber, A.; Thomas, S.; Burnley, P. C.

2012-12-01

The Berkeley Texture Package BEARTEX is a Windows-based computer software that combines various algorithms to analyze lattice-preferred orientation in polycrystalline materials. BEARTEX was initially designed to interpret diffraction intensity data from pole figure goniometers. Recently it has been successfully used to process synthetic forsterite powder diffraction data from in-situ synchrotron X-ray diffraction taken during deformation (Bollinger et al. 2012). Our study aims to test the practicability of using BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz (novaculite) during deformation. In-situ X-ray diffraction data was collected during the deformation of novaculite at 2.5 GPa and up to 1000 °C in a D-DIA apparatus using the ten-element energy-dispersive detector at the NSLS beamline X17B2. Diffraction intensities are a function of crystal orientation, expressed in azimuth angle η and pole distance ψ. The latter is the angle between the normal of a given diffraction plane and the vertical direction of the D-DIA apparatus - our principal stress direction during compression. Orientation-dependent diffraction intensities were corrected for different responses of the single detectors and x-ray absorption effects of the anvils. Orientation distributions (ODs) and inverse pole figures were calculated using BEARTEX. In addition, electron backscatter diffraction (EBSD) analyses were carried out on the deformed novaculite samples. Generated pole figures were compared with those derived from BEARTEX. Textural properties of our novaculite starting material complicated the BEARTEX analyses. The relatively strong variation of grain sizes in our natural specimens caused non-random diffraction intensity distributions. Those lead to non-random distributions of crystal orientations when analyzed with BEARTEX, although pole figures from EBSD data clearly show random crystal orientations. In an attempt to solve this problem, we employed a scanning routine when recording in-situ synchrotron X-ray diffraction and so collected diffraction from multiple sample volumes rather than from one single spot. Here, we will present a comparison of pole figures derived from independent BEARTEX and EBSD analyses for a series of novaculite experiments and discuss the practicability of BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz. REFERENCES C. BOLLINGER, S. MERKEL AND P. RATERRON (2012): In situ quantitative analysis of stress and texture development in forsterite aggregates deformed at 6 GPa and 1373 K. J. Appl. Cryst., 45, 263-271.

Experimental and theoretical investigations of non-centrosymmetric 8-hydroxyquinolinium dibenzoyl-(L)-tartrate methanol monohydrate single crystal

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

Sudharsana, N.; Krishnakumar, V.; Nagalakshmi, R., E-mail: nagaphys@yahoo.com

Graphical abstract: ORTEP diagram of HQDBT. - Highlights: • Single crystal XRD and NMR studies confirm the formation of the title compound. • SHG efficiency was found to be 0.6 times that of KDP. • First-order hyperpolarizability (β) was calculated using HF and B3LYP methods. - Abstract: A novel 8-hydroxyquinolinium dibenzoyl-(L)-tartrate methanol monohydrate crystal has been grown by slow evaporation technique. The single crystal X-ray diffraction analysis has been done for the title compound and is found to crystallize in orthorhombic space group P2{sub 1}2{sub 1}2{sub 1}. The optical absorption cut-off wavelength is found to be 440 nm. The vibrationalmore » analysis has been carried out to assess the functional groups present in the title compound. The molecular structure of the title compound has been confirmed by nuclear magnetic resonance spectroscopy. Thermogravimetric, differential scanning calorimetric and differential thermal analyses reveal the melting point and thermal stability of the title compound. The second harmonic generation efficiency is confirmed by Kurtz–Perry powder technique. Further quantum chemical calculations are performed using Gaussian 03 software.« less

A study of mercuric iodide near melting using differential scanning calorimetry, Raman spectroscopy and X-ray diffraction

NASA Astrophysics Data System (ADS)

Burger, A.; Morgan, S.; Jiang, H.; Silberman, E.; Schieber, M.; Van Den Berg, L.; Keller, L.; Wagner, C. N. J.

1989-11-01

High-temperature studies of mercuric iodide (HgI2) involving differential scanning calorimetry (DSC), Raman spectroscopy and X-ray powder diffraction have failed to confirm the existence of a red-colored tetragonal high-temperature phase called α'-HgI2 reported by S.N. Toubektsis et al. [J. Appl. Phys. 58 (1988) 2070] using DSC measurements. The multiple DSC peaks near melting reported by Toubektsis are found by the present authors only if the sample is heated in a stainless-steel container. Using a Pyrex container or inserting a platinum foil between the HgI2 and the stainless-steel container yields only one sharp, single DSC peak at the melting point. The nonexistence of the α' phase is confirmed by high-temperature X-ray diffraction and Raman spectroscopy performed in the vicinity of the melting point. These methods clearly, indicate the existence of only the yellow orthorhombic β-HgI2 phase. The experimental high-temperature DSC, Raman and X-ray diffraction data are presented and discussed.

Structured illumination multimodal 3D-resolved quantitative phase and fluorescence sub-diffraction microscopy

PubMed Central

Chowdhury, Shwetadwip; Eldridge, Will J.; Wax, Adam; Izatt, Joseph A.

2017-01-01

Sub-diffraction resolution imaging has played a pivotal role in biological research by visualizing key, but previously unresolvable, sub-cellular structures. Unfortunately, applications of far-field sub-diffraction resolution are currently divided between fluorescent and coherent-diffraction regimes, and a multimodal sub-diffraction technique that bridges this gap has not yet been demonstrated. Here we report that structured illumination (SI) allows multimodal sub-diffraction imaging of both coherent quantitative-phase (QP) and fluorescence. Due to SI’s conventionally fluorescent applications, we first demonstrate the principle of SI-enabled three-dimensional (3D) QP sub-diffraction imaging with calibration microspheres. Image analysis confirmed enhanced lateral and axial resolutions over diffraction-limited QP imaging, and established striking parallels between coherent SI and conventional optical diffraction tomography. We next introduce an optical system utilizing SI to achieve 3D sub-diffraction, multimodal QP/fluorescent visualization of A549 biological cells fluorescently tagged for F-actin. Our results suggest that SI has a unique utility in studying biological phenomena with significant molecular, biophysical, and biochemical components. PMID:28663887

Growth, structural, optical and thermal properties of gamma-glycine crystal.

PubMed

Balakrishnan, T; Babu, R Ramesh; Ramamurthi, K

2008-04-01

Single crystals of gamma-glycine were grown from a mixture of glycine, water and lithium bromide. Single crystal X-ray diffraction analysis confirmed the growth of gamma-glycine phase. Presence of various functional groups of gamma-glycine was identified by FTIR spectrum. Optical absorbance spectrum recorded in the wavelength range of UV-vis-NIR revealed that this crystal has good optical transparency in the range 250-1500 nm. Vickers microhardness values were estimated on the prominent (100) face. Thermogravimetric and differential scanning calorimetric analyses were carried out to study the thermal properties of gamma-glycine. Second harmonic generation efficiency of the crystal measured by Kurtz's powder method using Nd:YAG laser is about three times that of KDP.

Growth, structural, spectral, optical, and thermal studies on amino acid based new NLO single crystal: L-phenylalanine-4-nitrophenol.

PubMed

Prakash, M; Lydia Caroline, M; Geetha, D

2013-05-01

A new organic nonlinear optical single crystal, L-phenylalanine-4-nitrophenol (LPAPN) belonging to the amino acid group has been successfully grown by slow evaporation technique. The lattice parameters of the grown crystal have been determined by X-ray diffraction studies. FT-IR spectrum was recorded to identify the presence of functional group and molecular structure was confirmed by NMR spectrum. Thermal strength of the grown crystal has been studied using TG-DTA analyses. The grown crystals were found to be transparent in the entire visible region. The existence of second harmonic generation signals was observed using Nd:YAG laser with fundamental wavelength of 1064 nm. Copyright © 2013 Elsevier B.V. All rights reserved.

New Generation Agent Defeat Weapons: Energetic N,N'-Ethylene-Bridged Polyiodoazoles.

PubMed

Zhao, Gang; Kumar, Dheeraj; He, Chunlin; Hooper, Joseph P; Imler, Gregory H; Parrish, Damon A; Shreeve, Jean'ne M

2017-11-27

Sodium salts of iodine-rich pyrazole and imidazole with 1-(2-bromoethyl)-5-aminotetrazole are useful precursors for energetic N,N'-ethylene-bridged polyiodoazoles. Compounds 1-3 were characterized with IR, and 1 H and 13 C NMR spectroscopy as well as elemental analyses. The molecular structures of 1 and 2 were confirmed by using single crystal X-ray diffraction. Heats of formation were calculated using Gaussian 03 and detonation properties and biocidal efficiency were calculated with CHEETAH 7. The decomposition products of 1-3 destroy microbes more effectively than some previously reported biocides since the thermal decomposition occurs at below 400 °C without addition of oxidizer or combustion adjuvant. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analyse de l'état mécanique et microstructural de films minces supraconducteurs YBa_2 Cu_3O_7 par diffraction des rayons X

NASA Astrophysics Data System (ADS)

Auzary, S.; Badawi, K. F.; Bimbault, L.; Rabier, J.; Gaboriaud, R. J.; Goudeau, Ph.

1997-01-01

Mechanical and microstructural analysis in a 100nm thin film is presented in this study. Using X-ray diffraction with a tensorial approach, we have determined stresses, strains, stress-free lattice parameters, microdistorsions and diffracting coherent domains size. Stress-free lattice parameters are higher than the bulk values. A high value of stresses is explained as a combination of coherent stresses, thermal stresses and intrinsic ones. Diffraction peaks line profiles analysis suggests grain boundaries presence as well as high lattice elastic microdistorsions. Cette étude présente une analyse de l'état mécanique et microstructurale dans un film mince de 100nm d'épaisseur d'YBCO déposé sur un substrat de MgO. En utilisant la diffraction des rayons X couplée à une approche tensorielle, nous avons déterminé les déformations, les contraintes, les paramètres libres de contraintes, les microdistorsions élastiques ainsi que la taille des domaines cohérents de diffraction. Les paramètres libres de contrainte sont supérieurs à ceux du massif. Une valeur élevée des contraintes est expliquée à partir des contraintes de cohérence, des contraintes thermiques et intrinsèques. L'analyse des profils des pics de diffraction suggère la présence de sous-joints et de distorsions élastiques élevées au niveau des mailles cristallographiques.

Application of a real-space three-dimensional image reconstruction method in the structural analysis of noncrystalline biological macromolecules enveloped by water in coherent x-ray diffraction microscopy.

PubMed

Kodama, Wataru; Nakasako, Masayoshi

2011-08-01

Coherent x-ray diffraction microscopy is a novel technique in the structural analyses of particles that are difficult to crystallize, such as the biological particles composing living cells. As water is indispensable for maintaining particles in functional structures, sufficient hydration of targeted particles is required during sample preparation for diffraction microscopy experiments. However, the water enveloping particles also contributes significantly to the diffraction patterns and reduces the electron-density contrast of the sample particles. In this study, we propose a protocol for the structural analyses of particles in water by applying a three-dimensional reconstruction method in real space for the projection images phase-retrieved from diffraction patterns, together with a developed density modification technique. We examined the feasibility of the protocol through three simulations involving a protein molecule in a vacuum, and enveloped in either a droplet or a cube-shaped water. The simulations were carried out for the diffraction patterns in the reciprocal planes normal to the incident x-ray beam. This assumption and the simulation conditions corresponded to experiments using x-ray wavelengths of shorter than 0.03 Å. The analyses demonstrated that our protocol provided an interpretable electron-density map. Based on the results, we discuss the advantages and limitations of the proposed protocol and its practical application for experimental data. In particular, we examined the influence of Poisson noise in diffraction patterns on the reconstructed three-dimensional electron density in the proposed protocol.

Wigner analysis of three dimensional pupil with finite lateral aperture

PubMed Central

Chen, Hsi-Hsun; Oh, Se Baek; Zhai, Xiaomin; Tsai, Jui-Chang; Cao, Liang-Cai; Barbastathis, George; Luo, Yuan

2015-01-01

A three dimensional (3D) pupil is an optical element, most commonly implemented on a volume hologram, that processes the incident optical field on a 3D fashion. Here we analyze the diffraction properties of a 3D pupil with finite lateral aperture in the 4-f imaging system configuration, using the Wigner Distribution Function (WDF) formulation. Since 3D imaging pupil is finite in both lateral and longitudinal directions, the WDF of the volume holographic 4-f imager theoretically predicts distinct Bragg diffraction patterns in phase space. These result in asymmetric profiles of diffracted coherent point spread function between degenerate diffraction and Bragg diffraction, elucidating the fundamental performance of volume holographic imaging. Experimental measurements are also presented, confirming the theoretical predictions. PMID:25836443

Bis (3-methoxy-4-hydroxybenzaldehyde-2,4,6-trinitrophenol) organic cocrystal: Synthesis and physico-chemical properties

NASA Astrophysics Data System (ADS)

Sudharsana, N.; Krishnakumar, V.; Nagalakshmi, R.

2016-10-01

A 3-methoxy-4-hydroxybenzaldehyde-2,4,6-trinitrophenol (mhba-tnp) cocrystal was grown by the slow evaporation solution growth technique using ethanol as a solvent. As-grown crystals were characterized by single crystal X-ray diffraction (XRD) study and crystallized with a centrosymmetric space group. Optical properties of the grown crystal have been studied by Ultraviolet-Visible (UV-Vis) absorption spectra in the range from 200 to 800nm and the band gap energy of the crystal was obtained as 2.8eV. Fourier transform infrared (FTIR) and micro Raman spectral analyses have been carried out to confirm the functional groups present in the title compound. Differential scanning calorimetry (DSC) and polarized light thermomicroscopy (PLTM) analyses were carried out to find the melting point. In addition, the optimized geometric parameters and the molecular orbitals were calculated using density functional theory (DFT) with the help of the Gaussian 03W software.

Cu2SixSn1-xS3 Thin Films Prepared by Reactive Magnetron Sputtering For Low-Cost Thin Film Solar Cells

NASA Astrophysics Data System (ADS)

Yan, Chang; Liu, Fang-Yang; Lai, Yan-Qing; Li, Jie; Liu, Ye-Xiang

2011-10-01

We report the preparation of Cu2SixSn1-xS3 thin films for thin film solar cell absorbers using the reactive magnetron co-sputtering technique. Energy dispersive spectrometer and x-ray diffraction analyses indicate that Cu2Si1-xSnxS3 thin films can be synthesized successfully by partly substituting Si atoms for Sn atoms in the Cu2SnS3 lattice, leading to a shrinkage of the lattice, and, accordingly, by 2θ shifting to larger values. The blue shift of the Raman peak further confirms the formation of Cu2SixSn1-xS3. Environmental scanning electron microscope analyses reveal a polycrystalline and homogeneous morphology with a grain size of about 200-300 nm. Optical measurements indicate an optical absorption coefficient of higher than 104 cm-1 and an optical bandgap of 1.17±0.01 eV.

Radiation damage and annealing in plutonium tetrafluoride

DOE PAGES

McCoy, Kaylyn; Casella, Amanda; Sinkov, Sergey; ...

2017-08-03

A sample of plutonium tetrafluoride that was separated prior to 1966 at the Hanford Site in Washington State was analyzed at the Pacific Northwest National Laboratory (PNNL) in 2015 and 2016. The plutonium tetrafluoride, as received, was an unusual color and considering the age of the plutonium, there were questions about the condition of the material. These questions had to be answered in order to determine the suitability of the material for future use or long-term storage. Therefore, thermogravimetric/differential thermal analysis and X-ray diffraction evaluations were conducted to determine the plutonium's crystal structure, oxide content, and moisture content; these analysesmore » reported that the plutonium was predominately amorphous and tetrafluoride, with an oxide content near ten percent. Freshly fluorinated plutonium tetrafluoride is known to be monoclinic. And during the initial thermogravimetric/differential thermal analyses, it was discovered that an exothermic event occurred within the material near 414 °C. X-ray diffraction analyses were conducted on the annealed tetrafluoride. The X-ray diffraction analyses indicated that some degree of recrystallization occurred in conjunction with the 414 °C event. This commentary describes the series of thermogravimetric/differential thermal and X-ray diffraction analyses that were conducted as part of this investigation at PNNL.« less

Evolution of thermo-physical properties and annealing of fast neutron irradiated boron carbide

NASA Astrophysics Data System (ADS)

Gosset, Dominique; Kryger, Bernard; Bonal, Jean-Pierre; Verdeau, Caroline; Froment, Karine

2018-03-01

Boron carbide is widely used as a neutron absorber in most nuclear reactors, in particular in fast neutron ones. The irradiation leads to a large helium production (up to 1022/cm3) together with a strong decrease of the thermal conductivity. In this paper, we have performed thermal diffusivity measurements and X-ray diffraction analyses on boron carbide samples coming from control rods of the French Phenix LMFBR reactor. The burnups range from 1021 to 8.1021/cm3. We first confirm the strong decrease of the thermal conductivity at the low burnup, together with high microstructural modifications: swelling, large micro-strains, high defects density, and disordered-like material conductivity. We observe the microstructural parameters are highly anisotropic, with high micro-strains and flattened coherent diffracting domains along the (00l) direction of the hexagonal structure. Performing heat treatments up to high temperature (2200 °C) allows us to observe the material thermal conductivity and microstructure restoration. It then appears the thermal conductivity healing is correlated to the micro-strain relaxation. We then assume the defects responsible for most of the damage are the helium bubbles and the associated stress fields.

A comparative study of the Aurivillius phase ferroelectrics CaBi 4Ti 4O 15 and BaBi 4Ti 4O 15

NASA Astrophysics Data System (ADS)

Tellier, J.; Boullay, Ph.; Manier, M.; Mercurio, D.

2004-06-01

The room temperature structures of the four-layer Aurivillius phase ferroelectrics CaBi 4Ti 4O 15 and BaBi 4Ti 4O 15 are determined by means of single crystal X-ray diffraction. Regarding the CaBi 4Ti 4O 15 phase, in agreement with the tolerance factor, a significant deformation of the perovskite blocks is observed. The rotation system of the octahedra is typical from even layer Aurivillius phases and leads to the use of the space group A2 1am. For the BaBi 4Ti 4O 15 phase, only a weak variation with respect to the F2 mm space group can be suggested from single crystal X-ray diffraction. A significant presence of Ba atoms in the [ M2O 2] slabs is confirmed in agreement with the previous works but specific Ba 2+ and Bi 3+ sites have to be considered due to the large difference in bounding requirement of these cations. Possible origins for the ferroelectric relaxor behavior of the Ba-based compound are discussed in view of the presented structural analyses.

Structural, Morphological, Differential Scanning Calorimetric and Thermogravimetric Studies of Ball Milled Fe Doped Nanoscale La0.67Sr0.33MnO3 Manganite

NASA Astrophysics Data System (ADS)

Astik, Nidhi; Jha, Prafulla K.; Pratap, Arun

2018-03-01

The ball milling route has been used to produce the La0.67Sr0.33Mn0.85Fe0.15O3 (LSMFO) nanocrystalline sample from oxide precursors. The sample was characterized using x-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDAX), differential scanning calorimetry (DSC) and thermogravimetric (TGA) measurements. The x-ray diffraction confirms the phase purity of sample and shows that the sample crystallizes in the rhombohedral perovskite structure with a R-3c space group. The scanning electron micrograph shows the presence of well-faceted crystallites of LSMFO. The EDAX spectrum demonstrates the molar ratio of different elements of nanocrystalline LSMFO. Furthermore, the crystallite size using the Debye-Scherrer formula and William-Hall analysis has been found as 24 nm and 29 nm, respectively. Our results support the idea that a good quality nanocrystalline LSMFO sample can be obtained using the ball milling route. We also discuss the DSC and TGA curves and analyse the results in terms of phase transition, calcination temperature and activation barrier energies.

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

PubMed

Dinakaran, Paul M; Kalainathan, S

2013-07-01

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

Physical chemical effects of zinc on in vitro enamel demineralization.

PubMed

Mohammed, N R; Mneimne, M; Hill, R G; Al-Jawad, M; Lynch, R J M; Anderson, P

2014-09-01

Zinc salts are formulated into oral health products as antibacterial agents, yet their interaction with enamel is not clearly understood. The aim was to investigate the effect of zinc concentration [Zn(2+)] on the in vitro demineralization of enamel during exposure to caries-simulating conditions. Furthermore, the possible mechanism of zinc's action for reducing demineralization was determined. Enamel blocks and synthetic hydroxyapatite (HAp) were demineralized in a range of zinc-containing acidic solutions (0-3565ppm [Zn(2+)]) at pH 4.0 and 37°C. Inductively coupled-plasma optical emission spectroscopy (ICP-OES) was used to measure ion release into solution. Enamel blocks were analysed by Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy (ATR-FTIR), and HAp by X-ray diffraction (XRD) and neutron diffraction (ND). ICP-OES analysis of the acidic solutions showed a decrease in [Ca(2+)] and [PO4(3-)] release with increasing [Zn(2+)]. FTIR revealed a α-hopeite (α-Zn3(PO4)2.4H2O)-like phase on the enamel surfaces at >107ppm [Zn(2+)]. XRD and ND analysis confirmed a zinc-phosphate phase present alongside the HAp. This study confirms that zinc reduces enamel demineralization. Under the conditions studied, zinc acts predominantly on enamel surfaces at PO4(3-) sites in the HAp lattice to possibly form an α-hopeite-like phase. These results have a significant implication on the understanding of the fundamental chemistry of zinc in toothpastes and demonstrate its therapeutic potential in preventing tooth mineral loss. Copyright © 2014 The Authors. Published by Elsevier Ltd.. All rights reserved.

Stable diffraction-management soliton in a periodic structure with alternating left-handed and right-handed media

NASA Astrophysics Data System (ADS)

Zhang, Jinggui

2017-09-01

In this paper, we first derive a modified two-dimensional non-linear Schrödinger equation including high-order diffraction (HOD) suitable for the propagation of optical beam near the low-diffraction regime in Kerr non-linear media with spatial dispersion. Then, we apply our derived physical model to a designed two-dimensional configuration filled with alternate layers of a left-handed material (LHM) and a right-handed media by employing the mean-field theory. It is found that the periodic structure including LHM may experience diminished, cancelled, and even reversed diffraction behaviours through engineering the relative thickness between both media. In particular, the variational method analytically predicts that close to the zero-diffraction regime, such periodic structure can support stable diffraction-management solitons whose beamwidth and peak amplitude evolve periodically with the help of HOD effect. Numerical simulation based on the split-step Fourier method confirms the analytical results.

Fiber Diffraction Data Indicate a Hollow Core for the Alzheimer’s Aβ Three-fold Symmetric Fibril

PubMed Central

McDonald, Michele; Box, Hayden; Bian, Wen; Kendall, Amy; Tycko, Robert; Stubbs, Gerald

2012-01-01

Amyloid β protein (Aβ), the principal component of the extracellular plaques found in the brains of Alzheimer’s disease patients, forms fibrils well suited to structural study by X-ray fiber diffraction. Fiber diffraction patterns from the 40-residue form Aβ(1–40) confirm a number of features of a three-fold symmetric Aβ model from solid state NMR, but suggest that the fibrils have a hollow core, not present in the original ssNMR models. Diffraction patterns calculated from a revised hollow three-fold model with a more regular β-sheet structure are in much better agreement with the observed diffraction data than patterns calculated from the original ssNMR model. Refinement of a hollow-core model against ssNMR data led to a revised ssNMR model, similar to the fiber diffraction model. PMID:22903058

Organic Photonics: Toward a New Generation of Thin Film Photovoltaics and Lasers

DTIC Science & Technology

2011-03-07

plane. 39 Both electron and x - ray diffraction confirm the existence of crystalline domains of CuPc and C60. Crystalline domain sizes range from 5...nanocrystalline domains indicated by white curves that locate the domain boundaries. Scale bar=5 nm. b, X - ray diffraction pattern of an OVPD grown A... ray diffraction (XRD) and atomic force microscopy (AFM), as shown in Fig. 8. A cross-sectional TEM image of [CuPc(6.1nm)/C60(6.1nm)]10 is shown in

Publications - GMC 58 | Alaska Division of Geological & Geophysical Surveys

Science.gov Websites

DGGS GMC 58 Publication Details Title: X-ray diffraction and scanning electron microscopy mineral , Michael, and Core Laboratories, 1985, X-ray diffraction and scanning electron microscopy mineral analyses

Scalar limitations of diffractive optical elements

NASA Technical Reports Server (NTRS)

Johnson, Eric G.; Hochmuth, Diane; Moharam, M. G.; Pommet, Drew

1993-01-01

In this paper, scalar limitations of diffractive optic components are investigated using coupled wave analyses. Results are presented for linear phase gratings and fanout devices. In addition, a parametric curve is given which correlates feature size with scalar performance.

Quantitative assessment of image motion blur in diffraction images of moving biological cells

NASA Astrophysics Data System (ADS)

Wang, He; Jin, Changrong; Feng, Yuanming; Qi, Dandan; Sa, Yu; Hu, Xin-Hua

2016-02-01

Motion blur (MB) presents a significant challenge for obtaining high-contrast image data from biological cells with a polarization diffraction imaging flow cytometry (p-DIFC) method. A new p-DIFC experimental system has been developed to evaluate the MB and its effect on image analysis using a time-delay-integration (TDI) CCD camera. Diffraction images of MCF-7 and K562 cells have been acquired with different speed-mismatch ratios and compared to characterize MB quantitatively. Frequency analysis of the diffraction images shows that the degree of MB can be quantified by bandwidth variations of the diffraction images along the motion direction. The analytical results were confirmed by the p-DIFC image data acquired at different speed-mismatch ratios and used to validate a method of numerical simulation of MB on blur-free diffraction images, which provides a useful tool to examine the blurring effect on diffraction images acquired from the same cell. These results provide insights on the dependence of diffraction image on MB and allow significant improvement on rapid biological cell assay with the p-DIFC method.

Magneto-optical properties of BaCryFe12-yO19 (0.0 ≤ y ≤ 1.0) hexaferrites

NASA Astrophysics Data System (ADS)

Asiri, S.; Güner, S.; Korkmaz, A. D.; Amir, Md.; Batoo, K. M.; Almessiere, M. A.; Gungunes, H.; Sözeri, H.; Baykal, A.

2018-04-01

In this study, nanocrystalline BaCryFe12-yO19 (0.0 ≤ y ≤ 1.0) hexaferrite powders were prepared by sol-gel auto combustion method and the effect of Cr3+ ion substitution on morphology, structure, optic and magnetic properties of Barium hexaferrite were investigated. X-ray powder diffraction (XRD) analyses confirmed the purity of all samples. The XRD data shows that the average crystallite size lies between 60.95 nm and 50.10 nm and same was confirmed by Transmission electron microscopy. Transmission electron and scanning electron microscopy analyses presented the hexagonal morphology of all products. The characteristic hysteresis (σ-H) curves proved the ferromagnetic feature of as grown nanoparticle samples. Specific saturation magnetization (σs) drops from 46.59 to 34.89 emu/g with increasing Cr content while the coercive field values lie between 770 and 1652 Oe. The large magnitude of the magnetocrystalline (intrinsic) anisotropy field, (Ha) between 11.0 and 12.6 kOe proves that all products are magnetically hard. The energy band gap values decrease from 2.0 eV to 1.84 eV with increasing Cr content. From 57Fe Mössbauer spectroscopy, the variation in line width, isomer shift, quadrupole splitting and hyperfine magnetic field values were determined and discussed.

Comparative study of synthesis, structural and magnetic properties of Cu2+ substituted Co-Ni, Co-Zn and Co-Mg nano ferrites

NASA Astrophysics Data System (ADS)

Ramakrishna, A.; Murali, N.; Margarette, S. J.; Samatha, K.; Veeraiah, V.

2018-02-01

Mixed ferrites of the form Co0.5M0.1Cu0.4Fe2O4 (M = Ni, Zn and Mg) have been synthesized using the sol-gel auto combustion technique. Structural analyses are carried out using powder X-ray diffraction to idntify pure ferrite phases. SEM analysis revealed clear crystal morphology with relatively uniform grain sizes with polygonal structures. The FT-IR studies also confirm the bond formation and cation vibrations at low (365-392 cm-1) and high (579-587 cm-1) bands that correspond to the tetrahedral and octahedral sites, respectively. The magnetic properties studied through vibrating sample magnetometer showed that the Ni substituted sample has more magnetic character by exhibiting the highest saturation magnetization.

Catalytic properties of Co3O4 nanoparticles for rechargeable Li/air batteries.

PubMed

Kim, Kwan Su; Park, Yong Joon

2012-01-05

Three types of Co3O4 nanoparticles are synthesized and characterized as a catalyst for the air electrode of a Li/air battery. The shape and size of the nanoparticles are observed using scanning electron microscopy and transmission electron microscopy analyses. The formation of the Co3O4 phase is confirmed by X-ray diffraction. The electrochemical property of the air electrodes containing Co3O4 nanoparticles is significantly associated with the shape and size of the nanoparticles. It appears that the capacity of electrodes containing villiform-type Co3O4 nanoparticles is superior to that of electrodes containing cube- and flower-type Co3O4 nanoparticles. This is probably due to the sufficient pore spaces of the villiform-type Co3O4 nanoparticles.

Isobenzofuranones and Isochromenones from the Deep-Sea Derived Fungus Leptosphaeria sp. SCSIO 41005

PubMed Central

Luo, Xiaowei; Lin, Xiuping; Salendra, Limbadri; Pang, Xiaoyan; Dai, Yu; Yang, Bin; Liu, Juan; Wang, Junfeng; Liu, Yonghong

2017-01-01

Four new isobenzofuranones, leptosphaerins J–M (1–4), including an unusual naturally-occurring centrosymmetric dimer skeleton (1), and two new isochromenones, clearanols I–J (9–10), were obtained from a culture of a deep-sea sediment-derived fungus Leptosphaeria sp. SCSIO 41005, together with four known isobenzofuranones (5–8) and six known isochromenones (11–16). These structures were elucidated by extensive spectroscopic analyses, and absolute configurations were assigned on the basis of electronic circular dichroism and optical rotations data comparison. Additionally, the absolute configurations of the new compounds 1 and 9, together with the known one 7 with stereochemistry undetermined, were further confirmed by single crystal X-ray diffraction experiments. A plausible biosynthetic pathway of these isobenzofuranones and isochromenones was also proposed. PMID:28661451

Progression in structural, magnetic and electrical properties of La-doped group IV elements

NASA Astrophysics Data System (ADS)

Deepapriya, S.; Annie Vinosha, P.; Rodney, John D.; Jerome Das, S.

2018-04-01

Progression of group IV elements such as zinc ferrite (ZnFe2O4), cobalt ferrite (CoFe2O4) was synthesized by doping lanthanum (La), via adopting a facile co-precipitation method. Doping hefty rare earth ion in spinel structure can amend to the physical properties of the lattice, which can be used in the enhancement of magnetic and electrical properties of the as-synthesized nanomaterial, it is vital to metamorphose and optimize its micro structural and magnetic features. The structural properties of the samples was analysed by powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), Transmission electron microscopy (TEM) and UV-visible spectral analysis (UV-vis) reveals the optical property and optical band gap. The magnetic properties were evaluated using a vibrating sample magnetometer (VSM), the presence of functional group was confirmed by FTIR. XRD analyses elucidates that the synthesized samples zinc and cobalt had a spinel structure. From TEM analyses the morphology and diameter of the particle was observed. The substituted rare earth ions in Zinc ferrite inhibit the grain growth of the materials in an efficient manner compared with that of the Cobalt ferrite.

Creation of vector beams from a polarization diffraction grating using a programmable liquid crystal spatial light modulator and a q-plate

NASA Astrophysics Data System (ADS)

Badham, Katherine Emily

This thesis presents the ability of complete polarization control of light to create a polarization diffraction grating (PDG). This system has the ability to create diffracted light with each order having a separate high-order polarization state in one location on the optical axis. First, an external Excel program is used to create a grating phase profile from userspecified target diffraction orders. High-order vector beams in this PDG are created using a combination of two devices---a liquid crystal spatial light modulator (LC-SLM) manufactured by Seiko Epson, and a tunable q -plate from Citizen Holdings Co. The transmissive SLM is positioned in an optical setup with a reflective architecture allowing control over both the horizontal and vertical components of the laser beam. The SLM has its LC director oriented vertically only affecting the vertically polarized state, however, the optical setup allows modulation of both vertical and horizontal components by the use of a quarter-wave plate (QWP) and a mirror to rotate the polarizations 90 degrees. Each half of the SLM is encoded with an anisotropic phase-only diffraction grating which are superimposed to create a select number of orders with the desired polarization states and equally distributed intensity. The technique of polarimetry is used to confirm the polarization state of each diffraction order. The q-plate is an inhomogeneous birefringent waveplate which has the ability to convert zero-order vector beams into first-order vector beams. The physical placement of this device into the system converts the orders with zero-order polarization states to first-order polarization states. The light vector patterns of each diffraction order confirm which first-order polarization state of is produced. A specially made PDG sextuplicator is encoded onto the SLM to generate six diffraction orders with separate states of polarization.

JCPDS-ICDD Research Associateship (Cooperative Program with NBS/NIST)

PubMed Central

Wong-Ng, W.; McMurdie, H. F.; Hubbard, C. R.; Mighell, A. D.

2001-01-01

The Research Associateship program of the Joint Committee on Powder Diffraction-International Centre for Diffraction Data (JCPDS-ICDD, now known as the ICDD) at NBS/NIST was a long standing (over 35 years) successful industry-government cooperation. The main mission of the Associateship was to publish high quality x-ray reference patterns to be included in the Powder Diffraction File (PDF). The PDF is a continuing compilation of patterns gathered from many sources, compiled and published by the ICDD. As a result of this collaboration, more than 1500 high quality powder diffraction patterns, which have had a significant impact on the scientific community, were reported. In addition, various research collaborations with NBS/NIST also led to the development of several standard reference materials (SRMs) for instrument calibration and quantitative analyses, and computer software for data collection, calibration, reduction, for the editorial process of powder pattern publication, analysis of powder data, and for quantitative analyses. This article summarizes information concerning the JCPDS-ICDD organization, the Powder Diffraction File (PDF), history and accomplishments of the JCPDS-ICDD Research Associateship. PMID:27500061

Talbot effect of the defective grating in deep Fresnel region

NASA Astrophysics Data System (ADS)

Teng, Shuyun; Wang, Junhong; Zhang, Wei; Cui, Yuwei

2015-02-01

Talbot effect of the grating with different defect is studied theoretically and experimentally in this paper. The defects of grating include the loss of the diffraction unit, the dislocation of the diffraction unit and the modulation of the unit separation. The exact diffraction distributions of three kinds of defective gratings are obtained according to the finite-difference time-domain (FDTD) method. The calculation results show the image of the missing or dislocating unit appears at the Talbot distance (as mentioned in K. Patorski Prog. Opt., 27, 1989, pp.1-108). This is the so-called self-repair ability of grating imaging. In addition, some more phenomena are discovered. The loss or the dislocation of diffraction unit causes the diffraction distortion within a certain radial angle. The regular modulation of unit separation changes the original diffraction, but the new periodicity of the diffraction distribution rebuilds. The self-imaging of grating with smaller random modulation still keeps the partial self-repair ability, and yet this characteristic depends on the modulation degree of defective grating. These diffraction phenomena of the defective gratings are explained by use of the diffraction theory of grating. The practical experiment is also performed and the experimental results confirm the theoretic predictions.

Characterization and antimicrobial activity of silver nanoparticles, biosynthesized using Bacillus species

NASA Astrophysics Data System (ADS)

Ghiuță, I.; Cristea, D.; Croitoru, C.; Kost, J.; Wenkert, R.; Vyrides, I.; Anayiotos, A.; Munteanu, D.

2018-04-01

In this work, the biosynthesis of silver nanoparticles, using AgNO3 as a precursor, by two Bacillus species, namely Bacillus amyloliquefaciens and Bacillus subtillis, is reported. After the synthesis stages, the absorbance of the brown nanoparticle colloidal solutions was assessed by UV-vis spectrophotometry, which showed the peak absorbance values at 418 nm and 414 nm, corresponding to surface plasmon resonance of silver nanoparticles. The EDX, SEM and DLS analyses confirmed the formation of spherical silver nanoparticles with an average diameter smaller than 140 nm. XRD confirmed the presence of face-centered cubic silver crystals, with the highest intensity peak at 2θ = 38.12°, which corresponds to the (111) diffraction planes. The antibacterial activity after 24 h of incubation was observed against gram negative bacteria: Escherichia coli, Pseudomonas aeruginosa, Salmonella, as well as gram positive: Staphylococcus aureus, Streptococcus pyogenes. Furthermore, the antifungal activity was assessed against Candida albicans. The inhibition zone was clearly observed on the plates containing silver nanoparticles, either standalone or in combination with antibiotics, thus showing their potentiating antibacterial effect.

Synthesis, structural and spectral characterization of a novel NLO crystal N,N‧-diphenylguanidinium picrate: diacetone solvate

NASA Astrophysics Data System (ADS)

Shanmugavadivu, T.; Dhandapani, M.; Naveen, S.; Lokanath, N. K.

2017-09-01

An organic NLO active material N,N‧-diphenylguanidinium picrate: diacetone solvate (C13H14N3+. C6H2N3O7-. 2C3H6O) (DPGPD) was synthesized and single crystals were grown by slow evaporation-solution growth technique at room temperature. DPGPD crystallizes in monoclinic crystal system with noncentrosymmetric space group, Cc confirmed by single crystal X-ray diffraction analysis. The presence of various functional groups was identified from FT-IR spectral analysis and the proton transfer during the formation of compound was confirmed by NMR spectroscopic techniques. The thermal stability was investigated by TG/DTA analyses. Optical transmittance was measured by UV-Vis-NIR spectroscopy and band gap energy was calculated. Photoluminescence spectrum was used to explore its applicability towards laser diodes. Dielectric property of the material was ascertained at different temperatures and it is found that the grown crystal has higher dielectric constant in low frequencies. Photoconductivity study revealed that DPGPD exhibits positive photoconductivity. SHG property was found to be 0.6 times higher than that of KDP.

Synthesis, growth, crystal structure, optical and third order nonlinear optical properties of quinolinium derivative single crystal: PNQI

NASA Astrophysics Data System (ADS)

Karthigha, S.; Krishnamoorthi, C.

2018-03-01

An organic quinolinium derivative nonlinear optical (NLO) crystal, 1-ethyl-2-[2-(4-nitro-phenyl)-vinyl]-quinolinium iodide (PNQI) was synthesized and successfully grown by slow evaporation solution growth technique. Formation of a crystalline compound was confirmed by single crystal X-ray diffraction. The quinolinium compound PNQI crystallizes in the triclinic crystal system with a centrosymmetric space group of P-1 symmetry. The molecular structure of PNQI was confirmed by 1H NMR and 13C NMR spectral studies. The thermal properties of the crystal have been investigated by thermogravimetric (TG) and differential scanning calorimetry (DSC) studies. The optical characteristics obtained from UV-Vis-NIR spectral data were described and the cut-off wavelength observed at 506 nm. The etching study was performed to analyse the growth features of PNQI single crystal. The third order NLO properties such as nonlinear refractive index (n2), nonlinear absorption coefficient (β) and nonlinear susceptibility (χ (3)) of the crystal were investigated using Z-scan technique at 632.8 nm of Hesbnd Ne laser.

The effect of reaction temperature on the room temperature ferromagnetic property of sol-gel derived tin oxide nanocrystal

NASA Astrophysics Data System (ADS)

Sakthiraj, K.; Hema, M.; Balachandra Kumar, K.

2018-06-01

In the present study, nanocrystalline tin oxide materials were prepared using sol-gel method with different reaction temperatures (25 °C, 50 °C, 75 °C & 90 °C) and the relation between the room temperature ferromagnetic property of the sample with processing temperature has been analysed. The X-ray diffraction pattern and infrared absorption spectra of the as-prepared samples confirm the purity of the samples. Transmission electron microscopy images visualize the particle size variation with respect to reaction temperature. The photoluminescence spectra of the samples demonstrate that luminescence process in materials is originated due to the electron transition mediated by defect centres. The room temperature ferromagnetic property is observed in all the samples with different amount, which was confirmed using vibrating sample magnetometer measurements. The saturation magnetization value of the as-prepared samples is increased with increasing the reaction temperature. From the photoluminescence & magnetic measurements we accomplished that, more amount of surface defects like oxygen vacancy and tin interstitial are created due to the increase in reaction temperature and it controls the ferromagnetic property of the samples.

Polarization-induced interfacial coupling modulations in BaTiO3/GaN heterojunction devices

NASA Astrophysics Data System (ADS)

Bhat, Thirumaleshwara N.; Pandey, B. K.; Krupanidhi, S. B.

2017-07-01

We report on the ferroelectric polarization-induced switchable interfacial coupling modulations in BaTiO3/GaN heterojunction transport behaviour. The ferroelectric barium titanate, BaTiO3 (BTO) was integrated with polar semiconductor gallium nitride (GaN). BTO with a tetragonal structure was deposited on a wurtzite (0 0 0 1) epitaxial GaN/c-Al2O3 substrate by pulsed laser deposition, which was further confirmed by x-ray diffraction and Raman spectroscopy. BTO/GaN heterojunctions with resistive switching behaviour exhibited modulations in transport characteristics due to the interfacial coupling. The ferroelectric nature and interfacial coupling effect of this heterojunction was confirmed with the help of piezo-response force microscopy. A valence band offset of 0.82 eV and conduction band offset of 0.62 eV were obtained for BTO/GaN heterojunctions by x-ray photo-electron spectroscopy. This interfacial coupling phenomenon was analysed and its effect on the carrier conduction in the heterojunction was investigated by band alignment studies.

Characterization of Antibiotic-Loaded Alginate-Osa Starch Microbeads Produced by Ionotropic Pregelation

PubMed Central

Fontes, Gizele Cardoso; Calado, Verônica Maria Araújo; Rossi, Alexandre Malta; da Rocha-Leão, Maria Helena Miguez

2013-01-01

The aim of this study was to characterize the penicillin-loaded microbeads composed of alginate and octenyl succinic anhydride (OSA) starch prepared by ionotropic pregelation with calcium chloride and to evaluate their in vitro drug delivery profile. The beads were characterized by size, scanning electron microscopy (SEM), zeta potential, swelling behavior, and degree of erosion. Also, the possible interaction between penicillin and biopolymers was investigated by differential scanning calorimetry (DSC), powder X-ray diffraction (XRD), and Fourier transform infrared (FTIR) analysis. The SEM micrograph results indicated a homogeneous drug distribution in the matrix. Also, based on thermal analyses (TGA/DSC), interactions were detected between microbead components. Although FTIR spectra of penicillin-loaded microbeads did not reveal the formation of new chemical entities, they confirmed the chemical drug stability. XRD patterns showed that the incorporated crystalline structure of penicillin did not significantly alter the primarily amorphous polymeric network. In addition, the results confirmed a prolonged penicillin delivery system profile. These results imply that alginate and OSA starch beads can be used as a suitable controlled-release carrier for penicillin. PMID:23862146

A novel method to delaminate nitrate-intercalated MgAl layered double hydroxides in water and application in heavy metals removal from waste water.

PubMed

Rahman, Mir Tamzid; Kameda, Tomohito; Kumagai, Shogo; Yoshioka, Toshiaki

2018-07-01

Nitrate-intercalated MgAl layered double hydroxide (LDH) was successfully delaminated in water by a facile and effective method upon reflux at 120 °C for 24 h followed by sonication at 40 °C for 5 h. This process is environmentally friendly since water is the only solvent used. The delaminated nanosheets were characterized by microscopic, spectroscopic, and particle size analyses. The delamination process successfully produced octahedron-shaped single-layer nanosheets 50-150 nm in size. X-ray photoelectron spectroscopy (XPS) data confirmed that the surface elements and their chemical status are consistent with the basic layer of MgAl LDH. The delaminated nanosheets displayed higher adsorption capacity for removing heavy metals from waste water than the original powdered LDH. After treating the waste water, a sharp and intense peak in the X-ray powder diffraction (XRD) pattern of the precipitate confirms the restacking of the LDH nanosheets. Copyright © 2018 Elsevier Ltd. All rights reserved.

Purification, crystallization and X-ray crystallographic analysis of a putative exopolyphosphatase from Zymomonas mobilis

PubMed Central

Zhang, Aili; Guo, Erhong; Qian, Lanfang; Tang, Nga-Yeung; Watt, Rory M.; Bartlam, Mark

2016-01-01

Exopolyphosphatase (PPX) enzymes degrade inorganic polyphosphate (poly-P), which is essential for the survival of microbial cells in response to external stresses. In this study, a putative exopolyphosphatase from Zymomonas mobilis (ZmPPX) was crystallized. Crystals of the wild-type enzyme diffracted to 3.3 Å resolution and could not be optimized further. The truncation of 29 amino acids from the N-terminus resulted in crystals that diffracted to 1.8 Å resolution. The crystals belonged to space group C2, with unit-cell parameters a = 122.0, b = 47.1, c = 89.5 Å, α = γ = 90, β = 124.5°. An active-site mutant that crystallized in the same space group and with similar unit-cell parameters diffracted to 1.56 Å resolution. One molecule was identified per asymmetric unit. Analytical ultracentrifugation confirmed that ZmPPX forms a dimer in solution. It was confirmed that ZmPPX possesses exopolyphosphatase activity against a synthetic poly-P substrate. PMID:26919520

Purification, crystallization and X-ray crystallographic analysis of a putative exopolyphosphatase from Zymomonas mobilis.

PubMed

Zhang, Aili; Guo, Erhong; Qian, Lanfang; Tang, Nga-Yeung; Watt, Rory M; Bartlam, Mark

2016-03-01

Exopolyphosphatase (PPX) enzymes degrade inorganic polyphosphate (poly-P), which is essential for the survival of microbial cells in response to external stresses. In this study, a putative exopolyphosphatase from Zymomonas mobilis (ZmPPX) was crystallized. Crystals of the wild-type enzyme diffracted to 3.3 Å resolution and could not be optimized further. The truncation of 29 amino acids from the N-terminus resulted in crystals that diffracted to 1.8 Å resolution. The crystals belonged to space group C2, with unit-cell parameters a = 122.0, b = 47.1, c = 89.5 Å, α = γ = 90, β = 124.5°. An active-site mutant that crystallized in the same space group and with similar unit-cell parameters diffracted to 1.56 Å resolution. One molecule was identified per asymmetric unit. Analytical ultracentrifugation confirmed that ZmPPX forms a dimer in solution. It was confirmed that ZmPPX possesses exopolyphosphatase activity against a synthetic poly-P substrate.

Obtaining and characterization of La0.8Sr0.2CrO3 perovskite by the combustion method

NASA Astrophysics Data System (ADS)

Morales Rivera, A. M.; Gómez Cuaspud, J. A.; López, E. Vera

2017-01-01

This research is focused on the synthesis and characterization of a perovskite oxide based on La0.8Sr0.2CrO3 system by the combustion method. The material was obtained in order to contribute to analyse the effect of synthesis route in the obtaining of advanced anodic materials for solid oxide fuel cells (SOFC). The obtaining of solid was achieved starting from corresponding nitrate dissolutions, which were polymerized by temperature effect in presence of citric acid. The solid precursor as a foam citrate was characterized by infrared (FTIR) and ultraviolet (UV) spectroscopy, confirming the effectiveness in synthesis process. The solid was calcined in oxygen atmosphere at 800°C and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive of X-ray spectroscopy (EDX) and solid state impedance spectroscopy (IS). Results confirm the obtaining of an orthorhombic solid with space group Pnma (62) and cell parameters a=5.4590Å, b=7.7310Å and c=5.5050Å. At morphological level the solid showed a heterogeneous distribution with an optimal correspondence with proposed and obtained stoichiometry. The electrical characterization, confirm a semiconductor behaviour with a value of 2.14eV Band-gap according with previous works.

Growth, structural, spectral, mechanical, thermal and dielectric characterization of phosphoric acid admixtured L-alanine (PLA) single crystals.

PubMed

Rose, A S J Lucia; Selvarajan, P; Perumal, S

2011-10-15

Phosphoric acid admixtured L-alanine (PLA) single crystals were grown successfully by solution method with slow evaporation technique at room temperature. Crystals of size 18 mm×12 mm×8 mm have been obtained in 28 days. The grown crystals were colorless and transparent. The solubility of the grown samples has been found out at various temperatures. The lattice parameters of the grown crystals were determined by X-ray diffraction technique. The reflection planes of the sample were confirmed by the powder X-ray diffraction study and diffraction peaks were indexed. Fourier transform infrared (FTIR) studies were used to confirm the presence of various functional groups in the crystals. UV-visible transmittance spectrum was recorded to study the optical transparency of grown crystal. The nonlinear optical (NLO) property of the grown crystal was confirmed by Kurtz-Perry powder technique and a study of its second harmonic generation efficiency in comparison with potassium dihydrogen phosphate (KDP) has been made. The mechanical strength of the crystal was estimated by Vickers hardness test. The grown crystals were subjected to thermo gravimetric and differential thermal analysis (TG/DTA). The dielectric behavior of the sample was also studied. Copyright © 2011 Elsevier B.V. All rights reserved.

Imaging whole Escherichia coli bacteria by using single-particle x-ray diffraction

NASA Astrophysics Data System (ADS)

Miao, Jianwei; Hodgson, Keith O.; Ishikawa, Tetsuya; Larabell, Carolyn A.; Legros, Mark A.; Nishino, Yoshinori

2003-01-01

We report the first experimental recording, to our knowledge, of the diffraction pattern from intact Escherichia coli bacteria using coherent x-rays with a wavelength of 2 Å. By using the oversampling phasing method, a real space image at a resolution of 30 nm was directly reconstructed from the diffraction pattern. An R factor used for characterizing the quality of the reconstruction was in the range of 5%, which demonstrated the reliability of the reconstruction process. The distribution of proteins inside the bacteria labeled with manganese oxide has been identified and this distribution confirmed by fluorescence microscopy images. Compared with lens-based microscopy, this diffraction-based imaging approach can examine thicker samples, such as whole cultured cells, in three dimensions with resolution limited only by radiation damage. Looking forward, the successful recording and reconstruction of diffraction patterns from biological samples reported here represent an important step toward the potential of imaging single biomolecules at near-atomic resolution by combining single-particle diffraction with x-ray free electron lasers.

In situ investigation of deformation mechanisms in magnesium-based metal matrix composites

NASA Astrophysics Data System (ADS)

Farkas, Gergely; Choe, Heeman; Máthis, Kristián; Száraz, Zoltán; Noh, Yoonsook; Trojanová, Zuzanka; Minárik, Peter

2015-07-01

We studied the effect of short fibers on the mechanical properties of a magnesium alloy. In particular, deformation mechanisms in a Mg-Al-Sr alloy reinforced with short alumina fibers were studied in situ using neutron diffraction and acoustic emission methods. The fibers' plane orientation with respect to the loading axis was found to be a key parameter, which influences the acting deformation processes, such as twinning or dislocation slip. Furthermore, the twinning activity was much more significant in samples with parallel fiber plane orientation, which was confirmed by both acoustic emission and electron backscattering diffraction results. Neutron diffraction was also used to assist in analyzing the acoustic emission and electron backscattering diffraction results. The simultaneous application of the two in situ methods, neutron diffraction and acoustic emission, was found to be beneficial for obtaining complementary datasets about the twinning and dislocation slip in the magnesium alloys and composites used in this study.

STRUCTURE OF POTASSIUM HYDROGEN MALEATE BY NEUTRON DIFFRACTION

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

Peterson, S.W.; Levy, H.A.

1958-10-01

The preliminary results of a neutron diffraction study are presented which confirm the existence in potassium hydrogen maleate of a short, strong, hydrogen bond and show the ion to be at least statistically symmetrical. The hydrogen is strongly linked to both neighboring oxygen atoms, and there is an existing mode of correlated motion of considerable amplitude in which the oxygen atoms are displaced but hydrogen is not. (J.R.D.)

The Molecular Architecture for the Intermediate Filaments of Hard α -Keratin Based on the Superlattice Data Obtained from a Study of Mammals Using Synchrotron Fibre Diffraction

DOE PAGES

James, Veronica

2011-01-01

High- and low-angle X-ray diffraction studies of hard α -keratin have been studied, and various models have been proposed over the last 70 years. Most of these studies have been confined to one or two forms of alpha keratin. This high- and low-angle synchrotron fibre diffraction study extends the study to cover all available data for all known forms of hard α -keratin including hairs, fingernails, hooves, horn, and quills from mammals, marsupials, and a monotreme, and it confirms that the model proposed is universally acceptable for all mammals. A complete Bragg analysis of the meridional diffraction patterns, including multiple-timemore » exposures to verify any weak reflections, verified the existence of a superlattice consisting of two infinite lattices and three finite lattices. An analysis of the equatorial patterns establishes the radii of the oligomeric levels of dimers, tetramers, and intermediate filaments (IFs) together with the centre to centre distance for the IFs, thus confirming the proposed helices within helices molecular architecture for hard α -keratin. The results verify that the structure proposed by Feughelman and James meets the criteria for a valid α -keratin structure.« less

The Molecular Architecture for the Intermediate Filaments of Hard [alpha]-Keratin Based on the Superlattice Data Obtained from a Study ofMammals Using Synchrotron Fibre Diffraction

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

James, Veronica

2014-09-24

High- and low-angle X-ray diffraction studies of hard {alpha}-keratin have been studied, and various models have been proposed over the last 70 years. Most of these studies have been confined to one or two forms of alpha keratin. This high- and low-angle synchrotron fibre diffraction study extends the study to cover all available data for all known forms of hard {alpha}-keratin including hairs, fingernails, hooves, horn, and quills from mammals, marsupials, and a monotreme, and it confirms that the model proposed is universally acceptable for all mammals. A complete Bragg analysis of the meridional diffraction patterns, including multiple-time exposures tomore » verify any weak reflections, verified the existence of a superlattice consisting of two infinite lattices and three finite lattices. An analysis of the equatorial patterns establishes the radii of the oligomeric levels of dimers, tetramers, and intermediate filaments (IFs) together with the centre to centre distance for the IFs, thus confirming the proposed helices within helices molecular architecture for hard {alpha}-keratin. The results verify that the structure proposed by Feughelman and James meets the criteria for a valid {alpha}-keratin structure.« less

The Molecular Architecture for the Intermediate Filaments of Hard α -Keratin Based on the Superlattice Data Obtained from a Study of Mammals Using Synchrotron Fibre Diffraction

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

James, Veronica

High- and low-angle X-ray diffraction studies of hard α -keratin have been studied, and various models have been proposed over the last 70 years. Most of these studies have been confined to one or two forms of alpha keratin. This high- and low-angle synchrotron fibre diffraction study extends the study to cover all available data for all known forms of hard α -keratin including hairs, fingernails, hooves, horn, and quills from mammals, marsupials, and a monotreme, and it confirms that the model proposed is universally acceptable for all mammals. A complete Bragg analysis of the meridional diffraction patterns, including multiple-timemore » exposures to verify any weak reflections, verified the existence of a superlattice consisting of two infinite lattices and three finite lattices. An analysis of the equatorial patterns establishes the radii of the oligomeric levels of dimers, tetramers, and intermediate filaments (IFs) together with the centre to centre distance for the IFs, thus confirming the proposed helices within helices molecular architecture for hard α -keratin. The results verify that the structure proposed by Feughelman and James meets the criteria for a valid α -keratin structure.« less

Dynamical electron diffraction simulation for non-orthogonal crystal system by a revised real space method.

PubMed

Lv, C L; Liu, Q B; Cai, C Y; Huang, J; Zhou, G W; Wang, Y G

2015-01-01

In the transmission electron microscopy, a revised real space (RRS) method has been confirmed to be a more accurate dynamical electron diffraction simulation method for low-energy electron diffraction than the conventional multislice method (CMS). However, the RRS method can be only used to calculate the dynamical electron diffraction of orthogonal crystal system. In this work, the expression of the RRS method for non-orthogonal crystal system is derived. By taking Na2 Ti3 O7 and Si as examples, the correctness of the derived RRS formula for non-orthogonal crystal system is confirmed by testing the coincidence of numerical results of both sides of Schrödinger equation; moreover, the difference between the RRS method and the CMS for non-orthogonal crystal system is compared at the accelerating voltage range from 40 to 10 kV. Our results show that the CMS method is almost the same as the RRS method for the accelerating voltage above 40 kV. However, when the accelerating voltage is further lowered to 20 kV or below, the CMS method introduces significant errors, not only for the higher-order Laue zone diffractions, but also for zero-order Laue zone. These indicate that the RRS method for non-orthogonal crystal system is necessary to be used for more accurate dynamical simulation when the accelerating voltage is low. Furthermore, the reason for the increase of differences between those diffraction patterns calculated by the RRS method and the CMS method with the decrease of the accelerating voltage is discussed. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Application of Chlorophyll as Sensitizer for ZnS Photoanode in a Dye-Sensitized Solar Cell (DSSC)

NASA Astrophysics Data System (ADS)

Panda, B. B.; Mahapatra, P. K.; Ghosh, M. K.

2018-03-01

Zinc sulphide thin films have been synthesized by the electrodeposition method onto stainless steel substrate followed by dipping in acetone solution of chlorophyll in different time intervals to form photosensitised thin films. The photoelectrochemical parameters of the films have been studied using the photoelectrochemical cell having the cell configuration as follows {{photoelectrode/NaOH}}({1{{M}}} ) + {{S}}({1{{M}}} ) + {{N}}{{{a}}_2}{{S}}({1{{M}}} ){{/C}} ({{{graphite}}} ) . The photoelectrochemical characterization of the semiconductor film and dye-sensitised films has been carried out by measuring current-voltage (I-V) in the dark, power output and photoresponse. The study proves that the conductivity of both ZnS film and dye-sensitised ZnS films are n-type. The power output curves illustrate that open circuit voltage (V oc) and short circuit current (I sc) increase from 0.210 V to 0.312 V and from 0.297 mA to 0.533 mA, respectively. The fill factor initially decreases from 0.299 to 0.213 and then increases to 0.297 irregularly whereas efficiency increases from 0.047% to 0.123%. The UV-Vis absorbance spectrum of chlorophyll in acetone shows the presence of chlorophyll. The structural morphology of the ZnS thin films has also been analysed by using x-ray diffraction technique (XRD) and a scanning electron microscope (SEM). The XRD pattern shows the formation of nanocrystalline ZnS thin films of size 65 nm and the SEM images confirm the formation of fibrous film of ZnS. The energy diffraction analysis of x-ray confirms the formation of ZnS thin films.

A novel material of cross-linked styrylpyridinium salt intercalated montmorillonite for drug delivery

PubMed Central

2014-01-01

A facile synthesis of a styrylpyridinium salt (SbQ)/montmorillonite (MMT) via cationic exchange interactions between styrylpyridinium species (specifically SbQ) and MMT platelets is reported in this work. The SbQ-MMT solutions were irradiated under ultraviolet (UV) light for a specific time to obtain the cross-linked SbQ-MMT materials. Scanning electron microscopy and atomic force microscopy analyses revealed the structures and morphologies of MMT and modified MMT. X-ray diffraction and transmission electron microscope analyses indicated that the basal spacing increased from 1.24 to 1.53 nm compared with the pristine MMT, which proved that SbQ had interacted with MMT. Thermal gravimetric analysis curves showed that the amount of SbQ in the MMT interlayers was 35.71 meq/100 g. Fourier transform infrared spectroscopy also confirmed the intercalation of SbQ species into MMT interlayers, and UV spectroscopy was used to follow up the cross-linking of SbQ-MMT. This novel material has potential applications in drug delivery, and it can also be used as an additive to improve the mechanical properties of polymers. PMID:25170328

Preparation, Structural and Dielectric Properties of Solution Grown Polyvinyl Alcohol(PVA) Film

NASA Astrophysics Data System (ADS)

Nangia, Rakhi; Shukla, Neeraj K.; Sharma, Ambika

2017-08-01

Flexible dielectrics with high permittivity have been investigated extensively due to their applications in electronic industry. In this work, structural and electrical characteristics of polymer based film have been analysed. Poly vinyl alcohol (PVA) film was prepared by solution casting method. X-ray diffraction (XRD) characterization technique is used to investigate the structural properties. The semi-crystalline nature has been determined by the analysis of the obtained XRD pattern. Electrical properties of the synthesized film have been analysed from the C-V and I-V curves obtained at various frequencies and temperatures. Low conductivity values confirm the insulating behaviour of the film. However, it is found that conductivity increases with temperature. Also, the dielectric permittivity is found to be higher at lower frequencies and higher temperatures, that proves PVA to be an excellent dielectric material which can be used in interface electronics. Dielectric behaviour of the film has been explained based on dipole orientations to slow and fast varying electric field. However further engineering can be done to modulate the structural, electrical properties of the film.

Amorphous Calcium Carbonate Precipitation by Cellular Biomineralization in Mantle Cell Cultures of Pinctada fucata

PubMed Central

Xiang, Liang; Kong, Wei; Su, Jingtan; Liang, Jian; Zhang, Guiyou; Xie, Liping; Zhang, Rongqing

2014-01-01

The growth of molluscan shell crystals is generally thought to be initiated from the extrapallial fluid by matrix proteins, however, the cellular mechanisms of shell formation pathway remain unknown. Here, we first report amorphous calcium carbonate (ACC) precipitation by cellular biomineralization in primary mantle cell cultures of Pinctada fucata. Through real-time PCR and western blot analyses, we demonstrate that mantle cells retain the ability to synthesize and secrete ACCBP, Pif80 and nacrein in vitro. In addition, the cells also maintained high levels of alkaline phosphatase and carbonic anhydrase activity, enzymes responsible for shell formation. On the basis of polarized light microscopy and scanning electron microscopy, we observed intracellular crystals production by mantle cells in vitro. Fourier transform infrared spectroscopy and X-ray diffraction analyses revealed the crystals to be ACC, and de novo biomineralization was confirmed by following the incorporation of Sr into calcium carbonate. Our results demonstrate the ability of mantle cells to perform fundamental biomineralization processes via amorphous calcium carbonate, and these cells may be directly involved in pearl oyster shell formation. PMID:25405357

Study of free radicals in gamma irradiated cellulose of cultural heritage materials using Electron Paramagnetic Resonance

NASA Astrophysics Data System (ADS)

Kodama, Yasko; Rodrigues, Orlando, Jr.; Garcia, Rafael Henrique Lazzari; Santos, Paulo de Souza; Vasquez, Pablo A. S.

2016-07-01

Main subject of this article was to study room temperature stable radicals in Co-60 gamma irradiated contemporary paper using Electron Paramagnetic Resonance spectrometer (EPR). XRD was used to study the effect of ionizing radiation on the morphology of book paper. SEM images presented regions with cellulose fibers and regions with particles agglomeration on the cellulose fibers. Those agglomerations were rich in calcium, observed by EDS. XRD analysis confirmed presence of calcium carbonate diffraction peaks. The main objective of this study was to propose a method using conventional kinetics chemical reactions for the observed radical formed by ionizing radiation. Therefore, further analyses were made to study the half-life and the kinetics of the free radical created. This method can be suitably applied to study radicals on cultural heritage objects.

Energy and Biocides Storage Compounds: Synthesis and Characterization of Energetic Bridged Bis(triiodoazoles).

PubMed

He, Chunlin; Zhao, Gang; Hooper, Joseph P; Shreeve, Jean'ne M

2017-11-06

Energetic bridged triiodopyrazoles and triiodoimidazoles were designed and synthsized by reacting potassium triiodopyrazolate or triiodoimidazolate with corresponding dichloro compounds. All compounds were fully characterized by 1 H and 13 C NMR spectroscopy, IR spectroscopy, and elemental analyses. The structure of compound 1 was further confirmed by single-crystal X-ray diffraction. All of the compounds exhibit good thermal stability with decomposition temperatures between 199 and 270 °C and high densities ranging from 2.804 to 3.358 g/cm 3 . The detonation performances and the detonation products were calculated by CHEETAH 7. Compound 3 (D v = 4765 m s -1 ; P = 17.9 GPa) and compound 7 (D v = 4841 m s -1 ; P = 18.5 GPa) show comparable detonation pressure to TNT, and high iodine content makes them promising as energy and biocides storage compounds.

Synthesis and characterization of nanocomposite polymer blend electrolyte thin films by spin-coating method

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

Chapi, Sharanappa; Niranjana, M.; Devendrappa, H., E-mail: dehu2010@gmail.com

2016-05-23

Solid Polymer blend electrolytes based on Polyethylene oxide (PEO) and poly vinyl pyrrolidone (PVP) complexed with zinc oxide nanoparticles (ZnO NPs; Synthesized by Co-precipitation method) thin films have prepared at a different weight percent using the spin-coating method. The complexation of the NPs with the polymer blend was confirmed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR). The variation in film morphology was examined by polarized optical micrographs (POMs). The thermal behavior of blends was investigated under non-isothermal conditions by differential thermal analyses (DTA). A single glass transition temperature for each blend was observed, which supports the existence ofmore » compatibility of such system. The obtained results represent that the ternary based thin films are prominent materials for battery and optoelectronic device applications.« less

Fullerene-like Mo(W)(1-x)Re(x)S2 nanoparticles.

PubMed

Deepak, Francis Leonard; Popovitz-Biro, Ronit; Feldman, Yishay; Cohen, Hagai; Enyashin, Andrey; Seifert, Gotthard; Tenne, Reshef

2008-09-01

Inorganic fullerene-like (IF) Mo(1-x)Re(x)S(2) and W(1-x)Re(x)S(2) nanoparticles have been synthesized by a gas-phase reaction involving the respective metal halides with H(2)S. The IF-Mo(W)(1-x)Re(x)S(2) nanoparticles, containing up to 5 % Re, were characterized by a variety of experimental techniques. Analyses of the X-ray powder diffraction and different electron microscopy techniques show that the Re is doped in the MoS(2) host lattice. Interestingly, Re-doped MoS(2) nanotubes are present as well, although in small quantities ( approximately 5 %). XPS results confirm the nanoparticles to be more n-type arising from the effect of Re doping. Additionally, density-functional tight-binding (DFTB) calculations support the observed n-type behavior.

Bimetallic Cu-Ni nanoparticles supported on activated carbon for catalytic oxidation of benzyl alcohol

NASA Astrophysics Data System (ADS)

Kimi, Melody; Jaidie, Mohd Muazmil Hadi; Pang, Suh Cem

2018-01-01

A series of bimetallic copper-nickel (CuNix, x = 0.1, 0.2, 0.5 and 1) nanoparticles supported on activated carbon (AC) were prepared by deposition-precipitation method for the oxidation of benzyl alcohol to benzaldehyde using hydrogen peroxide as oxidising agent. Analyses by means of X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) confirmed that Cu and Ni was successfully added on the surface of activated carbon. CuNi1/AC showed the best catalytic activity for the oxidation of benzyl alcohols to the corresponding aldehyde within a short reaction period at 80 °C. The catalytic performance is significantly enhanced by the addition of equal amount of Ni as compared to the monometallic counterpart. This result indicates the synergistic effect between Ni and Cu particles in the catalytic oxidation reaction.

Frequency analysis for modulation-enhanced powder diffraction.

PubMed

Chernyshov, Dmitry; Dyadkin, Vadim; van Beek, Wouter; Urakawa, Atsushi

2016-07-01

Periodic modulation of external conditions on a crystalline sample with a consequent analysis of periodic diffraction response has been recently proposed as a tool to enhance experimental sensitivity for minor structural changes. Here the intensity distributions for both a linear and nonlinear structural response induced by a symmetric and periodic stimulus are analysed. The analysis is further extended for powder diffraction when an external perturbation changes not only the intensity of Bragg lines but also their positions. The derived results should serve as a basis for a quantitative modelling of modulation-enhanced diffraction data measured in real conditions.

Eco-friendly synthesis of Solanum trilobatum extract-capped silver nanoparticles is compatible with good antimicrobial activities

NASA Astrophysics Data System (ADS)

Ramanathan, Santheraleka; Gopinath, Subash C. B.; Anbu, Periasamy; Lakshmipriya, Thangavel; Kasim, Farizul Hafiz; Lee, Choul-Gyun

2018-05-01

This study focused on the evaluation of antimicrobial activity of silver nanoparticles (AgNPs) after their green synthesis by means of a Solanum trilobatum bark extract. The obtained product with an intense surface plasmon resonance band at ∼442 nm with UV-visible spectroscopic analysis indicated the formation of AgNPs. The morphology of AgNPs was observed under transmission electron microscopy and field emission scanning electron microscopy, displayed that the eco-friendly synthesized AgNPs have a spherical shape with an average size of ∼25 nm in diameter. X-ray powder diffraction and selected area electron diffraction analyses confirmed that the AgNPs are crystalline in nature. Fourier transform infrared spectroscopy indicated that the AgNPs capped with active ingredients of the bark extract. X-ray photoelectron spectroscopy revealed elemental composition of the AgNPs. The performance of S. trilobatum bark extract-capped AgNPs in terms of inhibition of microbial growth was studied by disc diffusion and well diffusion assays. Eco-friendly synthesized S. trilobatum extract-capped AgNPs were found to possess enhanced antimicrobial properties: growth inhibition of gram-negative and gram-positive bacteria and of fungal species. These results demonstrated the potential applications of the indigenous medicinal plants to the field of nanotechnology.

Roller compaction of different pseudopolymorphic forms of theophylline: Effect on compressibility and tablet properties.

PubMed

Hadzović, Ervina; Betz, Gabriele; Hadzidedić, Seherzada; El-Arini, Silvia Kocova; Leuenberger, Hans

2010-08-30

The effect of roller compaction on disintegration time, dissolution rate and compressibility of tablets prepared from theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate was studied. In addition, the influence of adding microcrystalline cellulose, a commonly used excipient, in mixtures with these materials was investigated. Theophylline anhydrate powder was used as a model drug to investigate the influence of different compaction pressures on the tablet properties. Tablets with same porosity were prepared by direct compaction and by roller compaction/re-compaction. Compressibility was characterized by Heckel and modified Heckel equations. Due to the property of polymorphic materials to change their form during milling and compression, X-ray diffraction analysis of theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate powders and granules was carried out. After roller compaction the disintegration time and the dissolution rate of the tablets were significantly improved. Compressibility of theophylline anhydrate powder and theophylline anhydrate fine powder was decreased, while theophylline monohydrate showed higher compressibility after roller compaction. Microcrystalline cellulose affected compressibility of theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate whereby the binary mixtures showed higher compressibility than the individual materials. X-ray diffraction analyses confirmed that there were no polymorphic/pseudopolymorphic changes after roller compaction. Copyright 2010 Elsevier B.V. All rights reserved.

Egg extract of apple snail for eco-friendly synthesis of silver nanoparticles and their antibacterial activity.

PubMed

Janthima, Ratima; Khamhaengpol, Arunrat; Siri, Sineenat

2018-03-01

Green synthesis of silver nanoparticles (AgNPs) provides the alternative method with cost effectiveness and the eco-friendly process by using natural biomolecules as reducing and stabilizing agents. Alternative to the most studies of plant extracts, this work demonstrated a use of egg extract of apple snail (Pomacea canaliculata) for an eco-friendly production of AgNPs. The extract contained at least six proteins with the molecular weight in a range of 24-65 kDa that exhibited the reducing activity. The dispersive AgNPs were produced in the reaction containing only the extract and silver nitrate, as determined by the characteristic surface plasmon resonance peak of silver at 412 nm. The synthesized AgNPs were spherical with the average diameter of 9.0 ± 5.9 nm. The X-ray diffraction pattern and selected area electron diffraction (SAED) analyses confirmed the face-cubic centre (fcc) unit cell structure of AgNPs. The synthesized AgNPs exhibited the antibacterial activity against both Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli. Results of this work clearly showed the potential use of the egg extract of apple snail for a green synthesis of small size AgNPs exhibiting the antibacterial activity.

Burgers Vector Analysis of Vertical Dislocations in Ge Crystals by Large-Angle Convergent Beam Electron Diffraction.

PubMed

Groiss, Heiko; Glaser, Martin; Marzegalli, Anna; Isa, Fabio; Isella, Giovanni; Miglio, Leo; Schäffler, Friedrich

2015-06-01

By transmission electron microscopy with extended Burgers vector analyses, we demonstrate the edge and screw character of vertical dislocations (VDs) in novel SiGe heterostructures. The investigated pillar-shaped Ge epilayers on prepatterned Si(001) substrates are an attempt to avoid the high defect densities of lattice mismatched heteroepitaxy. The Ge pillars are almost completely strain-relaxed and essentially defect-free, except for the rather unexpected VDs. We investigated both pillar-shaped and unstructured Ge epilayers grown either by molecular beam epitaxy or by chemical vapor deposition to derive a general picture of the underlying dislocation mechanisms. For the Burgers vector analysis we used a combination of dark field imaging and large-angle convergent beam electron diffraction (LACBED). With LACBED simulations we identify ideally suited zeroth and second order Laue zone Bragg lines for an unambiguous determination of the three-dimensional Burgers vectors. By analyzing dislocation reactions we confirm the origin of the observed types of VDs, which can be efficiently distinguished by LACBED. The screw type VDs are formed by a reaction of perfect 60° dislocations, whereas the edge types are sessile dislocations that can be formed by cross-slips and climbing processes. The understanding of these origins allows us to suggest strategies to avoid VDs.

Femtosecond diffraction dynamics of laser-induced periodic surface structures on fused silica

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

Hoehm, S.; Rosenfeld, A.; Krueger, J.

2013-02-04

The formation of laser-induced periodic surface structures (LIPSS) on fused silica upon irradiation with linearly polarized fs-laser pulses (50 fs pulse duration, 800 nm center wavelength) is studied experimentally using a transillumination femtosecond time-resolved (0.1 ps-1 ns) pump-probe diffraction approach. This allows to reveal the generation dynamics of near-wavelength-sized LIPSS showing a transient diffraction at specific spatial frequencies even before a corresponding permanent surface relief was observed. The results confirm that the ultrafast energy deposition to the materials surface plays a key role and triggers subsequent physical mechanisms such as carrier scattering into self-trapped excitons.

Discovery of a metastable Al20Sm4 phase

NASA Astrophysics Data System (ADS)

Ye, Z.; Zhang, F.; Sun, Y.; Mendelev, M. I.; Ott, R. T.; Park, E.; Besser, M. F.; Kramer, M. J.; Ding, Z.; Wang, C.-Z.; Ho, K.-M.

2015-03-01

We present an efficient genetic algorithm, integrated with experimental diffraction data, to solve a nanoscale metastable Al20Sm4 phase that evolves during crystallization of an amorphous magnetron sputtered Al90Sm10 alloy. The excellent match between calculated and experimental X-ray diffraction patterns confirms an accurate description of this metastable phase. Molecular dynamic simulations of crystal growth from the liquid phase predict the formation of disordered defects in the devitrified crystal.

Magnetic and thermal behavior of a family of compositionally related zero-dimensional fluorides

NASA Astrophysics Data System (ADS)

Felder, Justin B.; Smith, Mark D.; Sefat, Athena; zur Loye, Hans-Conrad

2018-07-01

The mild hydrothermal crystal growth technique has been leveraged to synthesize four new zero-dimensional transition metal fluorides. Their structures were determined by single crystal X-ray diffraction and confirmed by powder X-ray diffraction. The thermal, optical, and magnetic properties were investigated and the presence of thermal polymorphism and antiferromagnetism were observed. In addition, the potential application of these materials as precursors for advanced functional materials was explored.

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

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

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorptionmore » edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.« less

Component analyses of urinary nanocrystallites of uric acid stone formers by combination of high-resolution transmission electron microscopy, fast Fourier transformation, energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared spectroscopy.

PubMed

Sun, Xin-Yuan; Xue, Jun-Fa; Xia, Zhi-Yue; Ouyang, Jian-Ming

2015-06-01

This study aimed to analyse the components of nanocrystallites in urines of patients with uric acid (UA) stones. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, high-resolution transmission electron microscopy (HRTEM), fast Fourier transformation (FFT) of HRTEM, and energy dispersive X-ray spectroscopy (EDS) were performed to analyse the components of these nanocrystallites. XRD and FFT showed that the main component of urinary nanocrystallites was UA, which contains a small amount of calcium oxalate monohydrate and phosphates. EDS showed the characteristic absorption peaks of C, O, Ca and P. The formation of UA stones was closely related to a large number of UA nanocrystallites in urine. A combination of HRTEM, FFT, EDS and XRD analyses could be performed accurately to analyse the components of urinary nanocrystallites.

Mineralogy of a perudic Andosol in central Java, Indonesia

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

Van Ranst, Eric; Utami, S. R.; Verdoodt, A.

2008-02-15

We studied the mineralogy of a perudic Andosol developed on the Dieng Tephra Sequence in central Java, Indonesia. The objective was to confirm the presence and determine the origin and stability of 2:1 and interlayered 2:1 phyllosilicates in well-drained Andosols. This was and still is a debated topic in the literature. Total elemental and selective dissolution, as well as microscopic and X-ray diffraction analyses, were performed on the soil samples collected from this site. These analyses confirmed that andic properties were present in the soil samples. The allophane content determined by selective dissolution was 3-4% in the A horizons, andmore » increased to 12-18% in the deeper subsoil horizons. In addition, the clay fraction contained dioctahedral smectite, hydroxy-Al-interlayered 2:1 minerals (HIS), Al-chlorite, kaolinite, pyrophyllite, mica, cristobalite and some gibbsite. The silt and sand fractions were rich in plagioclase and pyroxene. The 2:1 minerals (smectite and pyrophyllite), as well as chlorite and kaolinite were of hydrothermal origin and were incorporated in the tephra during volcanic eruption. Besides desilication during dissolution of unstable minerals, Al interlayering of 2:1 layer silicates was most likely the most prominent pedogenic process. Although hydroxy-Al polymeric interlayers would normally stabilize the 2:1 clay phases, the strong weakening, and even disappearance of the characteristic XRD peaks, indicated instability of these minerals in the upper A horizons due to the perudic and intensive leaching conditions.« less

Mineralogy by X-ray Diffraction on Mars: The Chemin Instrument on Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Bristow, T. F.; Bish, D. L.; Ming, D. W.; Blake, D. F.; Morris, R. V.; Rampe, E. B.; Chipera, S. J.; Treiman, A. H.; Morrison, S. M.;

An extended UTD analysis for the scattering and diffraction from cubic polynomial strips

NASA Technical Reports Server (NTRS)

Constantinides, E. D.; Marhefka, R. J.

1993-01-01

Spline and polynomial type surfaces are commonly used in high frequency modeling of complex structures such as aircraft, ships, reflectors, etc. It is therefore of interest to develop an efficient and accurate solution to describe the scattered fields from such surfaces. An extended Uniform Geometrical Theory of Diffraction (UTD) solution for the scattering and diffraction from perfectly conducting cubic polynomial strips is derived and involves the incomplete Airy integrals as canonical functions. This new solution is universal in nature and can be used to effectively describe the scattered fields from flat, strictly concave or convex, and concave convex boundaries containing edges. The classic UTD solution fails to describe the more complicated field behavior associated with higher order phase catastrophes and therefore a new set of uniform reflection and first-order edge diffraction coefficients is derived. Also, an additional diffraction coefficient associated with a zero-curvature (inflection) point is presented. Higher order effects such as double edge diffraction, creeping waves, and whispering gallery modes are not examined. The extended UTD solution is independent of the scatterer size and also provides useful physical insight into the various scattering and diffraction processes. Its accuracy is confirmed via comparison with some reference moment method results.

On diamond, graphitic and amorphous carbons in primitive extraterrestrial solar system materials

NASA Technical Reports Server (NTRS)

Rietmeijer, Frans J. M.

1990-01-01

Carbon is among the most abundant elements in the universe and carbon chemistry in meteorites and comets is an important key to understanding many Solar System and interstellar processes. Yet, the mineralogical properties and interrelations between various structural forms of elemental carbon remain ambiguous. Crystalline elemental carbons include rhombohedral graphite, hexagonal graphite, cubic diamond, hexagonal diamond (i.e., lonsdaleite or carbon-2H) and chaoite. Elemental carbon also occurs as amorphous carbon and poorly graphitized (or turbostratic) carbon but of all the forms of elemental carbon only graphite is stable under physical conditions that prevail in small Solar System bodies and in the interstellar medium. The recent discovery of cubic diamond in carbonaceous chondrites and hexagonal diamond in chondritic interplanetary dust particles (IDPs) have created a renewed interest in the crystalline elemental carbons that were not formed by shock processes on a parent body. Another technique, Raman spectroscopy, confirms a widespread occurrence of disordered graphite in the Allende carbonaceous chondrite and in chondritic IDPs. Elemental carbons have also been identified by their characteristic K-edge features in electron energy loss spectra (EELS). However, the spectroscopic data do not necessarily coincide with those obtained by selected area electron diffraction (SAED). In order to interpret these data in terms of rational crystalline structures, it may be useful to consider the principles underlying electron diffraction and spectroscopic analyses. Electron diffraction depends on electron scattering, on the type of atom and the distance between atoms in a crystal lattice. Spectroscopic data are a function of the type of atom and the energy of bonds between atoms. Also, SAED is a bulk sampling technique when compared to techniques such as Raman spectroscopy or EELS. Thus, it appears that combined analyses provide contradictory results and that amorphous, or short-range ordered, carbon identified by conventional TEM imaging and SAED may show evidence for sp(3) bonds in EELS spectra. It is suggested that complex, nanometer-scale, mineralogical interrelations are common to all elemental carbons irrespective of their origin. The subsequent thermal history, or energy balance, will determine the ultimate microstructure.

Refraction effects in soft x-ray multilayer blazed gratings.

PubMed

Voronov, D L; Salmassi, F; Meyer-Ilse, J; Gullikson, E M; Warwick, T; Padmore, H A

2016-05-30

A 2500 lines/mm Multilayer Blazed Grating (MBG) optimized for the soft x-ray wavelength range was fabricated and tested. The grating coated with a W/B₄C multilayer demonstrated a record diffraction efficiency in the 2nd blazed diffraction order in the energy range from 500 to 1200 eV. Detailed investigation of the diffraction properties of the grating demonstrated that the diffraction efficiency of high groove density MBGs is not limited by the normal shadowing effects that limits grazing incidence x-ray grating performance. Refraction effects inherent in asymmetrical Bragg diffraction were experimentally confirmed for MBGs. The refraction affects the blazing properties of the MBGs and results in a shift of the resonance wavelength of the gratings and broadening or narrowing of the grating bandwidth depending on diffraction geometry. The true blaze angle of the MBGs is defined by both the real structure of the multilayer stack and by asymmetrical refraction effects. Refraction effects can be used as a powerful tool in providing highly efficient suppression of high order harmonics.

In-situ observation of recrystallization in an AlMgScZr alloy using confocal laser scanning microscopy

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

Taendl, J., E-mail: johannes.taendl@tugraz.atl; Nambu, S.; Orthacker, A.

2015-10-15

In this work we present a novel in-situ approach to study the recrystallization behavior of age hardening alloys. We use confocal laser scanning microscopy (CLSM) at 400 °C to investigate the static recrystallization of an AlMg4Sc0.4Zr0.12 alloy in-situ. The results are combined with electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) analyses. It was found that CLSM is a powerful tool to visualize both the local initiation and temporal sequence of recrystallization. After fast nucleation and initial growth, the grain growth rate decreases and the grain boundary migration stops after some minutes due to Zener pinning from Al{sub 3}(Sc,Zr)more » precipitates produced during the heat treatment. EBSD and TEM analyses confirm both the boundary movements and the particle-boundary interactions. - Highlights: • First time that CLSM is used to study recrystallization in-situ. • The start and end of recrystallization can be directly observed. • The procedure is easy to apply and requires only simple data interpretation. • In-situ observations on the surface correlate to modifications inside the bulk. • In-situ observations correlate to EBSD and EFTEM analyses.« less

Study of structural and optical properties of PbS thin films

NASA Astrophysics Data System (ADS)

Homraruen, T.; Sudswasd, Y.; Sorod, R.; Kayunkid, N.; Yindeesuk, W.

2018-03-01

This research aimed to synthesize lead sulfide (PbS) thin films on glass slides using the successive ion layer absorption and reaction (SILAR) method. We studied the optical properties and structure of PbS thin films by changing the number of dipping cycles and the concentration of precursor solution. The results of this experiment show that different conditions have a considerable influence on the thickness and absorbance of the films. When the number of dipping cycles and the concentration of the solution are increased, film thickness and absorbance tend to become higher. The xrays diffraction pattern showed all the diffraction peaks which confirmed the face center cubic and the structure of PbS had identified. Grain size computation was used to confirm how much these conditions could be affected.

Fabrication and investigation of effect of core size in heterostructure PbS/CdS core/shell nanoparticles

NASA Astrophysics Data System (ADS)

Das, D.; Hussain, A. M. P.

2018-04-01

PbS/CdS core/shell (CS) nanoparticles (NPs) were fabricated with three different concentrations of PbS core and CdS shell. Formation of core/shell heterostructure was confirmed from X-ray diffraction studies. The diffraction patterns exhibited formation of cubic phase and polycrystalline core/shell nanostructure. The crystalline sizes calculated from Williamson-Hall plot exhibited increase with molar concentration of precursors with decrease in strain. High resolution electron microscopy studies also confirm the formation of core/shell structure with particle size around 10 nm. A large blue-shift for PbS core compared to its bulk and small red-shift for the PbS/CdS core/shell as compared to the core is being observed in absorption spectra.

Fine Structure of Diffuse Scattering Rings in Al-Li-Cu Quasicrystal: A Comparative X-ray and Electron Diffraction Study

NASA Astrophysics Data System (ADS)

Donnadieu, P.; Dénoyer, F.

1996-11-01

A comparative X-ray and electron diffraction study has been performed on Al-Li-Cu icosahedral quasicrystal in order to investigate the diffuse scattering rings revealed by a previous work. Electron diffraction confirms the existence of rings but shows that the rings have a fine structure. The diffuse aspect on the X-ray diffraction patterns is then due to an averaging effect. Recent simulations based on the model of canonical cells related to the icosahedral packing give diffractions patterns in agreement with this fine structure effect. Nous comparons les diagrammes de diffraction des rayon-X et des électrons obtenus sur les mêmes échantillons du quasicristal icosaèdrique Al-Li-Cu. Notre but est d'étudier les anneaux de diffusion diffuse mis en évidence par un travail précédent. Les diagrammes de diffraction électronique confirment la présence des anneaux mais ils montrent aussi que ces anneaux possèdent une structure fine. L'aspect diffus des anneaux révélés par la diffraction des rayons X est dû à un effet de moyenne. Des simulations récentes basées sur la décomposition en cellules canoniques de l'empilement icosaédrique produisent des diagrammes de diffraction en accord avec ces effects de structure fine.

Photochemical quenching of aqueous methylene blue by N, Nb co-doped TiO2 nanomaterials under visible light: a confirmatory UV/LC-MS study

NASA Astrophysics Data System (ADS)

Gupta, Kamini; Pandey, Ashutosh; Singh, R. P.

2017-12-01

Nanodimensional un-doped, Nb doped, N doped and N,Nb co-doped TiO2 particles have been prepared by the sol-gel procedure. Phase identification of the anatase particles was done by X-ray powder diffraction and Deby-Scherrer calculations revealed their particle sizes to range from 20 to 30 nm. The band gap energies of the samples were measured by UV-Vis-diffuse reflectance (UV-DRS) spectra. While un-doped TiO2 showed wide optical absorption in the UV region. The co-doped TiO2 particles exhibited narrow band gaps of ~2.7 eV, which showed absorption in the visible region. A decline in charge carrier recombination rates in the prepared samples was confirmed through photoluminescence (PL). The morphological appearances of the particles have been examined by scanning electron microscopy. X-ray photoelectron spectroscopy (XPS) of the samples confirmed the incorporations of N and Nb into the TiO2 matrices. The photocatalytic efficiencies of the prepared particles have been determined by the degradation of the non-biodegradable dye methylene blue (MB) under electromagnetic radiation. The co-doped sample showed superior photocatalytic activity under the visible light (λ  >  400) over the other samples. Photochemical quenching of aqueous MB was further analysed by UV/LC-MS which confirmed the attenuation of methylene blue.

Experimental and density functional theory (DFT): A dual approach to probe the key properties of creatininium L-tartrate monohydrate single crystal for nonlinear optical applications

NASA Astrophysics Data System (ADS)

Thirumurugan, R.; Babu, B.; Anitha, K.; Chandrasekaran, J.

2017-12-01

A novel organic nonlinear optical (NLO) material, creatininium L-tartrate monohydrate (CTM) was synthesized and it was grown as single crystals with optical quality. 1H and 13C NMR spectral studies were performed and molecular structure of synthesized CTM compound was confirmed. Single crystal X-ray diffraction (SXRD) analysis confirmed that CTM was crystallized in orthorhombic system with non-centrosymmetric (NCS), P212121, space group. The grown crystal exhibited admirable properties such as second harmonic generation efficiency (SHG) (1.9 times KDP), and high laser damage threshold (LDT) value of 3.7 GW cm-2. CTM crystal displayed high transparency (∼60%) in the visible and near-IR region with low cut-off wavelength at 249 nm. Photoluminescence study confirmed blue wavelength emission (∼463 nm) of grown crystal. Thermal and mechanical behaviours have been successfully analysed for grown crystals. The dielectric studies were carried out for grown crystal as a function of frequencies at different temperatures. Hirshfeld surface and fingerprint plots provided the percentage of individual interactions contributed by each atom. Moreover, density functional theory (DFT) calculations have been employed to probe the frontier molecular orbitals (FMOs) and first hyperpolarizability (β) analysis of the optimized CTM structure. These results validated CTM as a suitable NLO candidate and were discussed in this work.

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

Zhao, Haishuang; Krysiak, Yaşar; Hoffmann, Kristin

The crystal structure and disorder phenomena of Al{sub 4}B{sub 2}O{sub 9}, an aluminum borate from the mullite-type family, were studied using automated diffraction tomography (ADT), a recently established method for collection and analysis of electron diffraction data. Al{sub 4}B{sub 2}O{sub 9}, prepared by sol-gel approach, crystallizes in the monoclinic space group C2/m. The ab initio structure determination based on three-dimensional electron diffraction data from single ordered crystals reveals that edge-connected AlO{sub 6} octahedra expanding along the b axis constitute the backbone. The ordered structure (A) was confirmed by TEM and HAADF-STEM images. Furthermore, disordered crystals with diffuse scattering along themore » b axis are observed. Analysis of the modulation pattern implies a mean superstructure (AAB) with a threefold b axis, where B corresponds to an A layer shifted by ½a and ½c. Diffraction patterns simulated for the AAB sequence including additional stacking disorder are in good agreement with experimental electron diffraction patterns. - Graphical abstract: Crystal structure and disorder phenomena of B-rich Al{sub 4}B{sub 2}O{sub 9} studied by automated electron diffraction tomography (ADT) and described by diffraction simulation using DISCUS. - Highlights: • Ab-initio structure solution by electron diffraction from single nanocrystals. • Detected modulation corresponding mainly to three-fold superstructure. • Diffuse diffraction streaks caused by stacking faults in disordered crystals. • Observed streaks explained by simulated electron diffraction patterns.« less

Growth and characterization of Methyl 2-amino-5-bromobenzoate crystal for NLO applications

NASA Astrophysics Data System (ADS)

Parthasarathy, M.; Gopalakrishnan, R.

2012-11-01

Good quality single crystal of organic Methyl 2-amino-5-bromobenzoate (M2A5B) was grown using slow evaporation solution growth technique. The grown crystal was confirmed by single crystal X-ray diffraction. The functional groups and vibrational frequencies were identified using FT-IR and FT-Raman spectral analyses. The presence of hydrogen and carbon atoms in the grown sample was confirmed with proton and carbon NMR spectral studies. The optical energy band gap of the title compound is found to be 2.7 eV from the optical transmission spectra. The refractive indices nx, ny, and nz were found to be 1.569, 1.587 and 1.600, respectively using Brewster's angle method. The melting point of the material obtained with melting point apparatus is 74 °C. Thermal stability of the grown crystal was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The mechanical behaviour of the grown crystal was analyzed with Vicker's microhardness tester. The particle size dependent second harmonic generation efficiency for M2A5B was evaluated by Kurtz-Perry powder method using Nd:YAG laser, which established the existence of phase matching.

Plasticity mechanism for copper extrusion in through-silicon vias for three-dimensional interconnects

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

Jiang, Tengfei; Spinella, Laura; Im, Jay

2013-11-18

In this paper, we demonstrated the plasticity mechanism for copper (Cu) extrusion in through-silicon via structures under thermal cycling. The local plasticity was directly observed by synchrotron x-ray micro-diffraction near the top of the via with the amount increasing with the peak temperature. The Cu extrusion was confirmed by Atomic Force Microscopy (AFM) measurements and found to be consistent with the observed Cu plasticity behavior. A simple analytical model elucidated the role of plasticity during thermal cycling, and finite element analyses were carried out to confirm the plasticity mechanism as well as the effect of the via/Si interface. The modelmore » predictions were able to account for the via extrusions observed in two types of experiments, with one representing a nearly free sliding interface and the other a strongly bonded interface. Interestingly, the AFM extrusion profiles seemed to contour with the local grain structures near the top of the via, suggesting that the grain structure not only affects the yield strength of the Cu and thus its plasticity but could also be important in controlling the pop-up behavior and the statistics for a large ensemble of vias.« less

Synthesis and Properties of a Clean and Sustainable Deicing Additive for Asphalt Mixture

PubMed Central

Peng, Chao; Yu, Jianying; Zhao, Zhijie; Dai, Jing; Fu, Jingyi; Zhao, Meiling; Wang, Wei

2015-01-01

A clean and sustainable deicing additive was prepared via the adsorption of acetate anions (Ac-) by magnesium (Mg) and aluminum (Al) calcined layered double hydroxide (Mg/Al-CLDH). Fourier transform infrared spectroscopy spectrums proved that Ac- had intercalated into LDH structure. X-ray diffraction patterns, scanning electron microscopy and transmission electron microscopy images showed that the intercalation spacing and platelet thickness of Mg and Al layered double hydroxide containing Ac- anions (Mg/Al-Ac- LDH) had been enlarged due to substitution of divalent CO3 2- anions by a larger quantity of monovalent Ac– anions. Differential scanning calorimetry tests testified that the insoluble Mg2/Al-Ac- LDH evidently decreased the freeze point (FP) of water to -10.68°C. X-ray photoelectron spectroscopy analyses confirmed that the Ac- were strongly confined by the metal layers of LDHs. FP test of asphalt mixtures confirmed that Mg/Al-Ac- LDHs reduced FP to -5.5°C. Immersion test results indicated that Mg/Al-Ac- LDH had a good deicing durability and Ac- did not released from asphalt mixture. Snow melting observation was conducted further testified that Mg/Al-Ac- LDH melted snow or ice sustainably. PMID:25625279

Synthesis and properties of a clean and sustainable deicing additive for asphalt mixture.

PubMed

Peng, Chao; Yu, Jianying; Zhao, Zhijie; Dai, Jing; Fu, Jingyi; Zhao, Meiling; Wang, Wei

2015-01-01

A clean and sustainable deicing additive was prepared via the adsorption of acetate anions (Ac-) by magnesium (Mg) and aluminum (Al) calcined layered double hydroxide (Mg/Al-CLDH). Fourier transform infrared spectroscopy spectrums proved that Ac- had intercalated into LDH structure. X-ray diffraction patterns, scanning electron microscopy and transmission electron microscopy images showed that the intercalation spacing and platelet thickness of Mg and Al layered double hydroxide containing Ac- anions (Mg/Al-Ac- LDH) had been enlarged due to substitution of divalent CO32- anions by a larger quantity of monovalent Ac- anions. Differential scanning calorimetry tests testified that the insoluble Mg2/Al-Ac- LDH evidently decreased the freeze point (FP) of water to -10.68°C. X-ray photoelectron spectroscopy analyses confirmed that the Ac- were strongly confined by the metal layers of LDHs. FP test of asphalt mixtures confirmed that Mg/Al-Ac- LDHs reduced FP to -5.5°C. Immersion test results indicated that Mg/Al-Ac- LDH had a good deicing durability and Ac- did not released from asphalt mixture. Snow melting observation was conducted further testified that Mg/Al-Ac- LDH melted snow or ice sustainably.

Characterization of bismuth selenide (Bi2Se3) thin films obtained by evaporating the hydrothermally synthesised nano-particles

NASA Astrophysics Data System (ADS)

Indirajith, R.; Rajalakshmi, M.; Gopalakrishnan, R.; Ramamurthi, K.

2016-03-01

Bismuth selenide (Bi2Se3) was synthesized by hydrothermal method at 200 °C and confirmed by powder X-ray diffraction (XRD) studies. The synthesized material was utilized to deposit bismuth selenide thin films at various substrate temperatures (Room Temperature-RT, 150 °C, 250 °C, 350 °C and 450 °C) by electron beam evaporation technique. XRD study confirmed the polycrystalline nature of the deposited Bi2Se3films. Optical transmittance spectra showed that the deposited (at RT) films acquire relatively high average transmittance of 60%in near infrared region (1500-2500 nm). An indirect allowed optical band gap calculated from the absorption edge for the deposited films is ranging from 0.62 to 0.8 eV. Scanning electron and atomic force microscopy analyses reveal the formation of nano-scale sized particles on the surface and that the nature of surface microstructures is influenced by the substrate temperature. Hall measurements showed improved electrical properties, for the films deposited at 350 °C which possess 2.8 times the mobility and 0.9 times the resistivity of the films deposited at RT.

The role of ultrasound in controlling the liquid-liquid phase separation and nucleation of vanillin polymorphs I and II

NASA Astrophysics Data System (ADS)

Parimaladevi, P.; Supriya, S.; Srinivasan, K.

2018-02-01

The influence of ultrasound on liquid-liquid phase separation (LLPS) and polymorphism of vanillin in aqueous solution has been investigated for the first time by varying the ultrasonic parameters such as power, pulse rate and insonation time at ambient condition. Results reveal that the application of ultrasound controls the impact of LLPS and accelerates the nucleation of vanillin within a short period at lower levels of ultrasonic process parameters, and also enhances the quality of the nucleated crystals. Moreover, the application of ultrasound induces the nucleation of rare and metastable polymorph of vanillin Form II in aqueous solution. But, at higher levels of power, pulse rate and insonation time, the rate of LLPS is found increased and the quality of the crystals becomes deteriorated. Morphology of the nucleated polymorphs were identified through optical microscopy and confirmed by optical goniometry. The internal structure and thermal stability of the grown stable Form I and metastable Form II of vanillin were confirmed through powder X-ray diffraction (PXRD) and differential scanning calorimetry (DSC) analyses. Further, results suggest that the ultrasound has profound effect in controlling the LLPS and nucleation of vanillin polymorphs in aqueous solution.

Growth, structural, optical, mechanical and quantum chemical analysis of unidirectional grown bis(guanidinium) 5-sulfosalicylate (BGSSA) single crystal

NASA Astrophysics Data System (ADS)

Sreedevi, R.; Saravana Kumar, G.; Amarsingh Bhabu, K.; Balu, T.; Murugakoothan, P.; Rajasekaran, T. R.

2018-02-01

Bis(guanidinium) 5-sulfosalicylate single crystal was grown by using Sankaranarayanan-Ramasamy (SR) method from the solution of methanol and water in equimolar ratio. Good quality crystal with 50 mm length and 10 mm in diameter was grown. The grown crystal was subjected to single crystal X-ray diffraction analysis to confirm the crystal structure and it was found to be orthorhombic. UV-Vis-NIR spectroscopic study revealed that the SR method grown crystal had good optical transparency with wide optical band gap of 4.4 eV. The presence of the functional groups and modes of vibrations were identified by FTIR spectroscopy recorded in the range 4000-400 cm-1. The mechanical strength of the grown crystal was confirmed using Vickers microhardness tester by applying load from 25 g to 100 g. Density functional theory (DFT) method with B3LYP/6-31-G (d,p) level basis set was employed and hence the optimized molecular geometry, first order hyperpolarizability, dipole moment, thermodynamic functions, molecular electrostatic potential and frontier molecular orbital analysis of the grown BGSSA sample was computed and analysed.

Evidence for the suppression of incident beam effects in Auger electron diffraction

NASA Astrophysics Data System (ADS)

Davoli, I.; Gunnella, R.; Bernardini, R.; De Crescenzi, M.

1998-01-01

Auger electron diffraction (AED) of the Cu(100) surface has been studied through the anisotropy of the elastic backdiffused beam electrons, the L 2,3M 4,5M 4,5 (LVV) and the M 2,3M 4,5M 4,5 (MVV) transitions in polar scan along the two main directions [001], [011] and in azimuth scan at normal emission. The intensity anisotropies of the low and high kinetic energy Auger lines are in antiphase to each other as in experiments in which these transitions are excited by X-ray photons. This behaviour has been exploited to single out the origin of the physical mechanisms accompanying the diffraction of the emitted electrons. Incident beam effects appear to be sizeable only when the collection of the AED spectra are made with an angle integrating electron analyser (cylindrical mirror analyser or low electron energy diffraction apparatus), but they appear negligible when electron collection is performed through a small solid-angle detector. The conclusions reached by our measurements are supported by good agreement with experimental and theoretical X-ray photoelectron diffraction data and demonstrate that, when the incident beam energy is sufficiently higher than the kinetic energy of the Auger electron detected, the influence of the incident beam on AED is negligible.

New software to model energy dispersive X-ray diffraction in polycrystalline materials

NASA Astrophysics Data System (ADS)

Ghammraoui, B.; Tabary, J.; Pouget, S.; Paulus, C.; Moulin, V.; Verger, L.; Duvauchelle, Ph.

2012-02-01

Detection of illicit materials, such as explosives or drugs, within mixed samples is a major issue, both for general security and as part of forensic analyses. In this paper, we describe a new code simulating energy dispersive X-ray diffraction patterns in polycrystalline materials. This program, SinFullscat, models diffraction of any object in any diffractometer system taking all physical phenomena, including amorphous background, into account. Many system parameters can be tuned: geometry, collimators (slit and cylindrical), sample properties, X-ray source and detector energy resolution. Good agreement between simulations and experimental data was obtained. Simulations using explosive materials indicated that parameters such as the diffraction angle or the energy resolution of the detector have a significant impact on the diffraction signature of the material inspected. This software will be a convenient tool to test many diffractometer configurations, providing information on the one that best restores the spectral diffraction signature of the materials of interest.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA.

PubMed

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-05-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the `diffraction before destruction' scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA

PubMed Central

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-01-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the ‘diffraction before destruction’ scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles. PMID:24763651

The science is in the data.

PubMed

Helliwell, John R; McMahon, Brian; Guss, J Mitchell; Kroon-Batenburg, Loes M J

2017-11-01

Understanding published research results should be through one's own eyes and include the opportunity to work with raw diffraction data to check the various decisions made in the analyses by the original authors. Today, preserving raw diffraction data is technically and organizationally viable at a growing number of data archives, both centralized and distributed, which are empowered to register data sets and obtain a preservation descriptor, typically a 'digital object identifier'. This introduces an important role of preserving raw data, namely understanding where we fail in or could improve our analyses. Individual science area case studies in crystallography are provided.

The science is in the data

PubMed Central

Kroon-Batenburg, Loes M. J.

2017-01-01

Understanding published research results should be through one’s own eyes and include the opportunity to work with raw diffraction data to check the various decisions made in the analyses by the original authors. Today, preserving raw diffraction data is technically and organizationally viable at a growing number of data archives, both centralized and distributed, which are empowered to register data sets and obtain a preservation descriptor, typically a ‘digital object identifier’. This introduces an important role of preserving raw data, namely understanding where we fail in or could improve our analyses. Individual science area case studies in crystallography are provided. PMID:29123672

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

PubMed

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

2014-01-24

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

Unique Chiral Interpenetrating d-f Heterometallic MOFs as Luminescent Sensors.

PubMed

Wu, Zhi-Lei; Dong, Jie; Ni, Wei-Yan; Zhang, Bo-Wen; Cui, Jian-Zhong; Zhao, Bin

2015-06-01

One novel three-dimensional (3D) 3d-4f metal-organic framework (MOF), [TbZn(L)(CO3)2(H2O)]n (1) [HL = 4'-(4-carboxyphenyl)-2,2':6',2″-terpyridine], has been successfully synthesized and structurally characterized. Structural analysis shows that compound 1 features a unique chiral interpenetrating 3D framework for the first time. The resulting crystals of 1 are composed of enantiomers 1a (P41) and 1b (P43), as was clearly confirmed by the crystal structure and the corresponding circular dichroism (CD) analyses of eight randomly selected crystals. The investigations on CD spectra based on every single crystal clearly assigned the Cotton effect signals. The powder X-ray diffraction measurement of 1 after being immersed in common solvents reveals that 1 possess excellent solvent stability. Furthermore, luminescent studies imply that 1 displays highly selective luminescent sensing of aldehydes, such as formol, acetaldehyde, and propanal.

Current induced polycrystalline-to-crystalline transformation in vanadium dioxide nanowires

PubMed Central

Jeong, Junho; Yong, Zheng; Joushaghani, Arash; Tsukernik, Alexander; Paradis, Suzanne; Alain, David; Poon, Joyce K. S.

2016-01-01

Vanadium dioxide (VO2) exhibits a reversible insulator-metal phase transition that is of significant interest in energy-efficient nanoelectronic and nanophotonic devices. In these applications, crystalline materials are usually preferred for their superior electrical transport characteristics as well as spatial homogeneity and low surface roughness over the device area for reduced scattering. Here, we show applied electrical currents can induce a permanent reconfiguration of polycrystalline VO2 nanowires into crystalline nanowires, resulting in a dramatically reduced hysteresis across the phase transition and reduced resistivity. Low currents below 3 mA were sufficient to cause the local temperature in the VO2 to reach about 1780 K to activate the irreversible polycrystalline-to-crystalline transformation. The crystallinity was confirmed by electron microscopy and diffraction analyses. This simple yet localized post-processing of insulator-metal phase transition materials may enable new methods of studying and fabricating nanoscale structures and devices formed from these materials. PMID:27892519

Detection of compatibility between baclofen and excipients with aid of infrared spectroscopy and chemometry

NASA Astrophysics Data System (ADS)

Rojek, Barbara; Wesolowski, Marek; Suchacz, Bogdan

2013-12-01

In the paper infrared (IR) spectroscopy and multivariate exploration techniques: principal component analysis (PCA) and cluster analysis (CA) were applied as supportive methods for the detection of physicochemical incompatibilities between baclofen and excipients. In the course of research, the most useful rotational strategy in PCA proved to be varimax normalized, while in CA Ward's hierarchical agglomeration with Euclidean distance measure enabled to yield the most interpretable results. Chemometrical calculations confirmed the suitability of PCA and CA as the auxiliary methods for interpretation of infrared spectra in order to recognize whether compatibilities or incompatibilities between active substance and excipients occur. On the basis of IR spectra and the results of PCA and CA it was possible to demonstrate that the presence of lactose, β-cyclodextrin and meglumine in binary mixtures produce interactions with baclofen. The results were verified using differential scanning calorimetry, differential thermal analysis, thermogravimetry/differential thermogravimetry and X-ray powder diffraction analyses.

Electrical properties of fullerenol C60(OH)10/Au interface

NASA Astrophysics Data System (ADS)

Sakaino, Masamichi; Sun, Yong; Morimoto, Fumio

2014-01-01

Electrical properties of the C60(OH)10/Au contact have been studied by measuring its current-voltage characteristics in the temperature range of 300-500 K. The Schottky barrier of the C60(OH)10/Au contact was confirmed to be 0.70±0.02 eV from Arrhenius plots of the current-voltage characteristics measured at various bias voltages as well as various preparation conditions of the C60(OH)10 material. Significant effect of the applied electric field on the barrier height has not been observed in the range of 0.1-2.0 MVm-1. The effects of both the charge transfer from C60 cage to OH groups and the crystallinity of the C60(OH)10 material on the Schottky barrier were discussed on the basis of x-ray photoemission spectroscopy and x-ray diffraction analyses.

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

PubMed

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

2014-02-01

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

Cold crucible induction melter test for crystalline ceramic waste form fabrication: A feasibility assessment

DOE PAGES

Amoroso, Jake W.; Marra, James; Dandeneau, Christopher S.; ...

2017-01-18

The first scaled proof-of-principle cold crucible induction melter (CCIM) test to process a multiphase ceramic waste form from a simulated combined (Cs/Sr, lanthanide and transition metal fission products) commercial used nuclear fuel waste stream was recently conducted in the United States. X-ray diffraction, 2-D X-ray absorption near edge structure (XANES), electron microscopy, inductively coupled plasma-atomic emission spectroscopy (and inductively coupled plasma-mass spectroscopy for Cs), and product consistency tests were used to characterize the fabricated CCIM material. Characterization analyses confirmed that a crystalline ceramic with a desirable phase assemblage was produced from a melt using a CCIM. We identified primary hollandite,more » pyrochlore/zirconolite, and perovskite phases in addition to minor phases rich in Fe, Al, or Cs. The material produced in the CCIM was chemically homogeneous and displayed a uniform phase assemblage with acceptable aqueous chemical durability.« less

Crocoite: An unusual mode of occurence for lead in coal

USGS Publications Warehouse

Li, Z.; Moore, T.A.; Weaver, S.D.; Finkelman, R.B.

2001-01-01

What is believed to be a very unusual mode of occurrence for lead in coal has been identified as crocoite (PbCrO4). As part of a larger study on trace elements and mineralogy in the Cretaceous Main Seam in New Zealand, crocoite was found in raw coal samples within the lower part of the coal seam. X-ray diffraction (XRD) and bulk chemical data from a SEM equipped with an energy dispersive X-ray analyser (EDXA) have confirmed the identity of this mineral. This is apparently the first time that crocoite has been reported in coal. Crocoite usually occurs only in the oxidised zone of lead mineral deposits. The occurrence of this mineral in the Main Seam coal implies that the deposit was exposed to an oxidising environment at some stage, most likely after coalification. Published by Elsevier Science B.V.

A biosensor system using nickel ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Singh, Prachi; Rathore, Deepshikha

2016-05-01

NiFe2O4 ferrite nanoparticles were synthesized by chemical co-precipitation method and the structural characteristics were investigated using X-ray diffraction technique, where single cubic phase formation of nanoparticles was confirmed. The average particle size of NiFe2O4 was found to be 4.9 nm. Nanoscale magnetic materials are an important source of labels for biosensing due to their strong magnetic properties which are not found in biological systems. This property of the material was exploited and the fabrication of the NiFe2O4 nanoparticle based biosensor was done in the form of a capacitor system, with NiFe2O4 as the dielectric material. The biosensor system was tested towards different biological materials with the help of electrochemical workstation and the same was analysed through Cole-Cole plot of NiFe2O4. The performance of the sensor was determined based on its sensitivity, response time and recovery time.

High temperature Ir segregation in Ir-B ceramics: Effect of oxygen presence on stability of IrB 2 and other Ir-B phases

DOE PAGES

Xie, Zhilin; Terracciano, Anthony C.; Cullen, David A.; ...

2015-05-13

The formation of IrB 2, IrB 1.35, IrB 1.1 and IrB monoboride phases in the Ir–B ceramic nanopowder was confirmed during mechanochemical reaction between metallic Ir and elemental B powders. The Ir–B phases were analysed after 90 h of high energy ball milling and after annealing of the powder for 72 h at 1050°C in vacuo. The iridium monoboride (IrB) orthorhombic phase was synthesised experimentally for the first time and identified by powder X-ray diffraction. Additionally, the ReB 2 type IrB 2 hexagonal phase was also produced for the first time and identified by high resolution transmission electron microscope. Irmore » segregation along disordered domains of the boron lattice was found to occur during high temperature annealing. Furthermore, these nanodomains may have useful catalytic properties.« less

8 MeV electron beam induced modifications in the thermal, structural and electrical properties of nanophase CeO2 for potential electronics applications

NASA Astrophysics Data System (ADS)

Babitha, K. K.; Sreedevi, A.; Priyanka, K. P.; Ganesh, S.; Varghese, Thomas

2018-06-01

The effect of 8 MeV electron beam irradiation on the thermal, structural and electrical properties of CeO2 nanoparticles synthesized by chemical precipitation route was investigated. The dose dependent effect of electron irradiation was studied using various characterization techniques such as, thermogravimetric and differential thermal analyses, X-ray diffraction, Fourier transformed infrared spectroscopy and impedance spectroscopy. Systematic investigation based on the results of structural studies confirm that electron beam irradiation induces defects and particle size variation on CeO2 nanoparticles, which in turn results improvements in AC conductivity, dielectric constant and loss tangent. Structural modifications and high value of dielectric constant for CeO2 nanoparticles due to electron beam irradiation make it as a promising material for the fabrication of gate dielectric in metal oxide semiconductor devices.

Effect of substrate temperature in the synthesis of BN nanostructures

NASA Astrophysics Data System (ADS)

Sajjad, M.; Zhang, H. X.; Peng, X. Y.; Feng, P. X.

2011-06-01

Boron nitride (BN) nanostructures were grown on molybdenum discs at different substrate temperatures using the short-pulse laser plasma deposition technique. Large numbers of randomly oriented nanorods of fiber-like structures were obtained. The variation in the length and diameter of the nanorods as a function of the substrate temperature was systematically studied. The surface morphologies of the samples were studied using scanning electron microscopy. Energy dispersive x-ray spectroscopy confirmed that both the elements boron and nitrogen are dominant in the nanostructure. The x-ray diffraction (XRD) technique was used to analyse BN phases. The XRD peak that appeared at 26° showed the presence of hexagonal BN phase, whereas the peak at 44° was related to cubic BN content in the samples. Raman spectroscopic analysis showed vibrational modes of sp2- and sp3-type bonding in the sample. The Raman spectra agreed well with XRD results.

Nano-crystalline hydroxyapatite bio-mineral for the treatment of strontium from aqueous solutions.

PubMed

Handley-Sidhu, Stephanie; Renshaw, Joanna C; Yong, Ping; Kerley, Robert; Macaskie, Lynne E

2011-01-01

Hydroxyapatites were analysed using electron microscopy, X-ray diffraction (XRD) and X-ray fluorescence (XRF) analysis. Examination of a bacterially produced hydroxyapatite (Bio-HA) by scanning electron microscopy showed agglomerated nano-sized particles; XRD analysis confirmed that the Bio-HA was hydroxyapatite, with an organic matter content of 7.6%; XRF analysis gave a Ca/P ratio of 1.55, also indicative of HA. The size of the Bio-HA crystals was calculated as ~25 nm from XRD data using the Scherrer equation, whereas Comm-HA powder size was measured as ≤ 50 μm. The nano-crystalline Bio-HA was ~7 times more efficient in removing Sr(2+) from synthetic groundwater than Comm-HA. Dissolution of HA as indicated by the release of phosphate into the solution phase was higher in the Comm-HA than the Bio-HA, indicating a more stable biomaterial which has a potential for the remediation of contaminated sites.

Structural and wetting properties of porous anodic alumina templates prepared by different electrolytes

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

Suchitra, S. M., E-mail: suchitra.ph14f03@nitk.edu.in; Reddy, P. Ramana; Udayashankar, N. K.

2016-05-06

Porous anodic alumina (PAA) has been extensively studied in recent years due to their unique properties and applications for manufacturing nanostructured materials. In this article, we report our studies on structural and wetting properties of PAA membranes prepared using different electrolytes such as sulphuric, oxalic and phosphoric acids. The morphological parameters such as pore diameter and porosity were measured using SEM and analysed using image-J software. The structural investigation of PAA membranes was carried out through X-ray diffraction analysis and it was confirmed that PAA membranes were amorphous in nature. The wetting behaviour of PAA membranes were measured using contactmore » angle measurement technique. The results show that PAA membranes were hydrophilic in nature with contact angles 26.03°, 35.21° and 42.0° for sulphuric, oxalic and phosphoric acids respectively.« less

Preservation of rodent bones from El Harhoura 2 cave (Morocco, Neolithic - Middle Palaeolithic): Microstructure, mineralogy, crystallinity and composition

NASA Astrophysics Data System (ADS)

Farre, Bastien; Massard, Pierre; Nouet, Julius; Dauphin, Yannicke

2014-04-01

Thin sections, scanning electron microscopy (SEM), diffraction X (DRX) and infrared spectrometry (FTIR) have been used to study the structure, mineralogy, crystallinity and bulk composition of fossil rodent long bones extracted from a succession of sedimentary layers in a cave from Morocco (Neolithic - Middle Palaeolithic, El Harhoura 2). The microstructure of fossil bones is well-preserved at this scale of observation, and encrusted deposits are rare. All bones are preserved in apatite, but the crystallinity is modified, as well as the crystallite shape, the organic content and the organic-mineral ratio. No fluor enrichment has been observed. Alone or together, the studied parameters do not show a regular trend from the upper to the lower layers of the cave. The preservation of the fossil bones does not confirm the sequence of arid and humid periods inferred from taphonomic analyses.

Solid-state reaction kinetics and optical studies of cadmium doped magnesium hydrogen phosphate crystals

NASA Astrophysics Data System (ADS)

Verma, Madhu; Gupta, Rashmi; Singh, Harjinder; Bamzai, K. K.

2018-04-01

The growth of cadmium doped magnesium hydrogen phosphate was successfully carried out by using room temperature solution technique i.e., gel encapsulation technique. Grown crystals were confirmed by single crystal X-ray diffraction (XRD). The structure of the grown crystal belongs to orthorhombic crystal system and crystallizes in centrosymmetric space group. Kinetics of the decomposition of the grown crystals were studied by non-isothermal analysis. Thermo gravimetric / differential thermo analytical (TG/DTA) studies revealed that the grown crystal is stable upto 119 °C. The various steps involved in the thermal decomposition of the material have been analysed using Horowitz-Metzger, Coats-Redfern and Piloyan-Novikova equations for evaluating various kinetic parameters. The optical studies shows that the grown crystals possess wide transmittance in the visible region and significant optical band gap of 5.5ev with cut off wavelength of 260 nm.

Characterization of potassium bromide crystals grown in the aqueous solution of picric acid

NASA Astrophysics Data System (ADS)

Maheswari, J. Uma; Krishnan, C.; Kalyanaraman, S.; Selvarajan, P.

2016-12-01

Potassium bromide crystals were grown in the aqueous solution of picric acid by slow evaporation technique at room temperature. X-ray Diffraction (XRD) analysis ensures that the grown sample is in Fm3m space group and FCC structure. Energy Dispersive X-ray Spectroscopy (EDX) reveals the presence of elements in the title compound. UV-Vis-NIR spectrum reveals that the grown sample is a promising nonlinear optical (NLO) material. FTIR analysis confirms the functional groups present in the sample. The thermogravimetric (TG) and differential thermogravimetric (DTA) analyses ensure that the sample material is thermally stable up to 160 °C. The second harmonic efficiency of the sample is 1.3 times greater than that of standard KDP. The mechanical strength of the grown sample is estimated by Vickers microhardness tester. The electrical properties were investigated by impedance analysis and the results of various studies of the grown crystals are discussed.

Synthesis, crystal structures, computational studies and antimicrobial activity of new designed bis((5-aryl-1,3,4-oxadiazol-2-yl)thio)alkanes

NASA Astrophysics Data System (ADS)

Ahmed, Muhammad Naeem; Sadiq, Beenish; Al-Masoudi, Najim A.; Yasin, Khawaja Ansar; Hameed, Shahid; Mahmood, Tariq; Ayub, Khurshid; Tahir, Muhammad Nawaz

2018-03-01

A new series of bis((5-aryl-1,3,4-oxadiazol-2-yl)thio)alkanes 4-14 have been synthesized via nucleophilic substitution reaction of dihaloalkanes with respective 1,3,4-oxadiazole-2-thiols 3a-f, and characterized by spectroscopic techniques. The structures of 4 and 12 were unambiguously confirmed by single-crystal X-ray diffraction analysis. Density functional theory calculations at B3LYP/6-31 + G(d) level of theory were performed for comparison of X-ray geometric parameters, molecular electrostatic potential (MEP) and frontier molecular orbital analyses of synthesized compounds. MEP analysis revealed that these compounds are nucleophilic in nature. Frontier molecular orbitals (FMOs) analysis of 4-14 was performed for evaluation of kinetic stability. All synthesized compounds were screened in vitro for antimicrobial activity against three bacterial and three fungal strains and showed promising results.

Pulsed laser deposition for the synthesis of monolayer WSe2

NASA Astrophysics Data System (ADS)

Mohammed, A.; Nakamura, H.; Wochner, P.; Ibrahimkutty, S.; Schulz, A.; Müller, K.; Starke, U.; Stuhlhofer, B.; Cristiani, G.; Logvenov, G.; Takagi, H.

2017-08-01

Atomically thin films of WSe2 from one monolayer up to 8 layers were deposited on an Al2O3 r-cut ( 1 1 ¯ 02 ) substrate using a hybrid-Pulsed Laser Deposition (PLD) system where a laser ablation of pure W is combined with a flux of Se. Specular X-ray reflectivities of films were analysed and were consistent with the expected thickness. Raman measurement and atomic force microscopy confirmed the formation of a WSe2 monolayer and its spatial homogeneity over the substrate. Grazing-incidence X-ray diffraction uncovered an in-plane texture in which WSe2 [ 10 1 ¯ 0 ] preferentially aligned with Al2O3 [ 11 2 ¯ 0 ]. These results present a potential to create 2D transition metal dichalcogenides by PLD, where the growth kinetics can be steered in contrast to common growth techniques like chemical vapor deposition and molecular beam epitaxy.

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.

Phase transition sequence in ferroelectric Aurivillius compounds investigated by single crystal X-ray diffraction

NASA Astrophysics Data System (ADS)

Boullay, P.; Tellier, J.; Mercurio, D.; Manier, M.; Zuñiga, F. J.; Perez-Mato, J. M.

2012-09-01

The investigation of the phase transition sequence in SrBi2Ta2O9 (SBT) and SrBi2Nb2O9 (SBN) is reported using single-crystal X-ray diffraction. By monitoring specific reflections as a function of temperature, sensitive either to the superstructure formation or to polar displacements, it was possible to check the existence or not of an intermediate phase. This latter was confirmed in SBT, but within experimental accuracy could not be detected in SBN.

The potential for the indirect crystal structure verification of methyl glycosides based on acetates' parent structures: GIPAW and solid-state NMR approaches

NASA Astrophysics Data System (ADS)

Szeleszczuk, Łukasz; Gubica, Tomasz; Zimniak, Andrzej; Pisklak, Dariusz M.; Dąbrowska, Kinga; Cyrański, Michał K.; Kańska, Marianna

2017-10-01

A convenient method for the indirect crystal structure verification of methyl glycosides was demonstrated. Single-crystal X-ray diffraction structures for methyl glycoside acetates were deacetylated and subsequently subjected to DFT calculations under periodic boundary conditions. Solid-state NMR spectroscopy served as a guide for calculations. A high level of accuracy of the modelled crystal structures of methyl glycosides was confirmed by comparison with published results of neutron diffraction study using RMSD method.

Analysis of x-ray diffraction pattern and complex plane impedance plot of polypyrrole/titanium dioxide nanocomposite: A simulation study

NASA Astrophysics Data System (ADS)

Ravikiran, Y. T.; Vijaya Kumari, S. C.

2013-06-01

To innovate the properties of Polypyrrole/Titanium dioxide (PPy/TiO2) nanocomposite further, it has been synthesized by chemical polymerization technique. The nanostructure and monoclinic phase of the prepared composite have been confirmed by simulating the X-ray diffraction pattern (XRD). Also, complex plane impedance plot of the composite has been simulated to find equivalent resistance capacitance circuit (RC circuit) and numerical values of R and C have been predicted.

An x-ray diffraction study of some mesoionic 2,3-diphenyltetrazoles

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

Luboradzki, R.; Kozminski, W.; Stefaniak, L.

1993-02-01

An X-my diffraction study is reported for four molecules of mesoionic 2,3-diphenyltetrazoles. The results confirm a dipolar [open quotes]mesoionic[close quotes] structure, aromatic character of the tetrazole ring and no conjugation between the phenyl and tetrazole rings. The geometry of the exocyclic group is discussed in detail. The molecular parameters of the compounds investigated are correlated with [sup 13]C and [sup 15]N nmr data. The results obtained are compared with similar structures which have already been studied.

Synthèses et supraconductivité de monocristaux à base de mercure

NASA Astrophysics Data System (ADS)

Pelloquin, D.; Villard, G.; Hardy, V.; Maignan, A.; Raveau, B.

1998-01-01

Single crystals (n = 1, 2 and 3) of the Hg_{l-x}M_xBa_2Ca_{n-1}Cu_n O_{2n+2+δ} mercury based cuprates have been grown by using a simple process. The M cations (M = Bi, Cu, Ti) act as stabilizers of the structure which permit to avoid the use of dry box or high gas pressure. The electron microscopy coupled with EDX analyses evidence the regularity of the stacking mode and confirm mixed mercury layers with compositions close to Hg_{0.8} M_{0.2}. Their structural studies based on X-ray diffraction data show a splitting of the oxygen site at the level of the mixed mercury layer. These as-grown superconducting single crystals exhibit T_c close to that of the corresponding pure mercury ceramics. The pinning properties study performed on (Hg_{0.8}Bi_{0.2}) crystals confirms that the n = 1 member is intermediate between the n = 2 and n = 3 members. Moreover, the weak properties of the Hg_{0.6}Ti_{0.4}{-}1223 crystals with regard to the Hg_{0.8}Bi_{0.2}{-}1223 crystals suggest that their different cationic radii Hg/M and their different c-axis values may play a role on these properties. Une méthode de synthèse simple, permettant de faire croître des monocristaux de composition Hg_{l-x}M_xBa_2Ca_{n-1}Cu_n O_{2n+2+δ} (n = 1, 2 et 3) sans utiliser de boîte à gants ou de techniques sous hautes pressions, a été developpée en substituant partiellement le mercure par un cation M (M = Bi, Cu, Ti). Des études par microscopie électronique couplées avec des analyses EDX ont confirmé les modes d'empilement et l'introduction de 1'é1ément M sous la forme de couches mixtes Hg_{0,8}M_{0,2}. Les études structurales réalisées par diffraction de rayons X sur monocristal ont mis en évidence un éclatement du site oxygène lié à la couche mercure. Ces monocristaux, bruts de synthèses, présentent des T_c comparables à celles observées dans les céramiques "tout mercure” correspondantes. L'étude des propriétés d'ancrage des vortex, menée sur les cristaux dopés au bismuth, confirme la position intermédiaire du terme n = 1 par rapport aux termes n = 2 et n = 3. De plus, une comparaison entre les cristaux de type 1223 (n = 3) dopés successivement au titane (Hg_{0,6}Ti_{0,4}{-}1223) et au bismuth (Hg_{0,8}Bi_{0,2}{-}1223) semble mettre en avant les valeurs du rapport Hg/M et du paramètre c sur ces propriétés.

Nuclear surface diffuseness revealed in nucleon-nucleus diffraction

NASA Astrophysics Data System (ADS)

Hatakeyama, S.; Horiuchi, W.; Kohama, A.

2018-05-01

The nuclear surface provides useful information on nuclear radius, nuclear structure, as well as properties of nuclear matter. We discuss the relationship between the nuclear surface diffuseness and elastic scattering differential cross section at the first diffraction peak of high-energy nucleon-nucleus scattering as an efficient tool in order to extract the nuclear surface information from limited experimental data involving short-lived unstable nuclei. The high-energy reaction is described by a reliable microscopic reaction theory, the Glauber model. Extending the idea of the black sphere model, we find one-to-one correspondence between the nuclear bulk structure information and proton-nucleus elastic scattering diffraction peak. This implies that we can extract both the nuclear radius and diffuseness simultaneously, using the position of the first diffraction peak and its magnitude of the elastic scattering differential cross section. We confirm the reliability of this approach by using realistic density distributions obtained by a mean-field model.

A Diffractive Reading of Dialogical Feedback through the Political Ethics of Care

ERIC Educational Resources Information Center

Bozalek, Vivienne; Mitchell, Veronica; Dison, Arona; Alperstein, Melanie

2016-01-01

With regard to improving higher education feedback practices, there is an increasing interest in using the efficacy of dialogue rather than the more traditional unidirectional approaches. We build on this impetus by considering how the ethics of care can be used to analyse the dialogical aspects of feedback. By diffractively reading insights of…

Facile and highly efficient approach for the fabrication of multifunctional silk nanofibers containing hydroxyapatite and silver nanoparticles.

PubMed

Sheikh, Faheem A; Ju, Hyung Woo; Moon, Bo Mi; Park, Hyun Jung; Kim, Jung-Ho; Lee, Ok Joo; Park, Chan Hum

2014-10-01

In this study, a good combination consisting of electrospun silk fibroin nanofibers incorporated with high-purity hydroxyapatite (HAp) nanoparticles (NPs) and silver NPs is introduced as antimicrobial for tissue engineering applications. The variable pressure field emission scanning electron microscope results confirmed randomly placed nanofibers are produced with highly dispersed HAp and silver NPs in nanofibers after electrospinning. The X-ray diffraction results demonstrated crystalline features of each of the three components used for electrospinning. Moreover, the TEM-EDS analysis confirmed the presence and chemical nature of each component over individual silk nanofiber. The FT-IR analyses was used confirm the different vibration modes caused due to functional groups present in silk fibroin, Hap, and silver NPs. The obtained nanofibers were checked for antimicrobial activity by using two model organisms Escherichia coli and Staphylococcus aureus. Subsequently, the antimicrobial tests have indicated that prepared nanofibers do possess good bactericidal activity. The ability of N,N-dimethylformamide and silk fibroin used to reduce silver nitrate into silver metal was evaluated using MTT assay. The nanofibers were grown in presence of NIH 3T3 fibroblasts, which revealed toxic behavior to fibroblasts at higher concentrations of silver nitrate used in this study. Furthermore, cell attachment studies on nanofibers for 3 and 12 days of incubation time were minutely observed and correlated with the results of MTT assay. The reported results confirmed the high amounts of silver nitrate can lead to toxic effects on viability of fibroblasts and had bad effect in cell attachment. © 2013 Wiley Periodicals, Inc.

Total-scattering pair-distribution function of organic material from powder electron diffraction data.

PubMed

Gorelik, Tatiana E; Schmidt, Martin U; Kolb, Ute; Billinge, Simon J L

2015-04-01

This paper shows that pair-distribution function (PDF) analyses can be carried out on organic and organometallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction and nanodiffraction in transmission electron microscopy or nanodiffraction in scanning transmission electron microscopy modes. The methods were demonstrated on organometallic complexes (chlorinated and unchlorinated copper phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering data and avoiding beam damage of the sample are possible to resolve.

Mechanical design of a precision linear flexural stage for 3D x-ray diffraction microscope at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Shu, D.; Liu, W.; Kearney, S.; Anton, J.; Tischler, J. Z.

2015-09-01

The 3-D X-ray diffraction microscope is a new nondestructive tool for the three-dimensional characterization of mesoscopic materials structure. A flexural-pivot-based precision linear stage has been designed to perform a wire scan as a differential aperture for the 3-D diffraction microscope at the Advanced Photon Source, Argonne National Laboratory. The mechanical design and finite element analyses of the flexural stage, as well as its initial mechanical test results with laser interferometer are described in this paper.

Single phase Pb0.7Bi0.3Fe0.65Nb0.35O3 multiferroic: Neutron diffraction, impedance and modulus studies

NASA Astrophysics Data System (ADS)

Dadami, Sunanda T.; Matteppanvar, Shidaling; Shivaraja, I.; Rayaprol, Sudhindra; Deshpande, S. K.; Angadi, Basavaraj

2018-04-01

The Pb0.7Bi0.3Fe0.65Nb0.35O3 (PBFNO) multiferroic solid solution was synthesized by using single step solid state reaction method. Single phase formation was confirmed through room temperature (RT) X Ray Diffraction (XRD) and Neutron Diffraction (ND). Rietveld refinement was used to perform the structural analysis using FullProf Suite program. RT XRD and ND patterns well fitted with monoclinic structure (Cm space group) and cell parameters from the ND data are found to be a = 5.6474(4) Å, b = 5.6415(3) Å, c = 3.9992(3) Å and β = 89.95(2)°. ND data at RT exhibits G-type antiferromagnetic structure. The electrical properties (impedance and modulus) of PBFNO were studied as a function of frequency (100 Hz - 5 MHz) and temperature (133 K - 293 K) by Impedance spectroscopy technique. Impedance and modulus spectroscopy studies confirm the contribution to the conductivity is from grains only and the relaxation is of non-Debye type. The PBFNO sample exhibits negative temperature coefficient of resistance (NTCR) behaviour. PBFNO is found be a potential candidate for RT applications.

Inflection point caustic problems and solutions for high-gain dual-shaped reflectors

NASA Technical Reports Server (NTRS)

Galindo-Israel, Victor; Veruttipong, Thavath; Imbriale, William; Rengarajan, Sembiam

1990-01-01

The singular nature of the uniform geometrical theory of diffraction (UTD) subreflector scattered field at the vicinity of the main reflector edge (for a high-gain antenna design) is investigated. It is shown that the singularity in the UTD edge-diffracted and slope-diffracted fields is due to the reflection distance parameter approaching infinity in the transition functions. While the geometrical optics (GO) and UTD edge-diffracted fields exhibit singularities of the same order, the edge slope-diffracted field singularity is more significant and is substantial for greater subreflector edge tapers. The diffraction analysis of such a subreflector in the vicinity of the main reflector edge has been carried out efficiently and accurately by a stationary phase evaluation of the phi-integral, whereas the theta-integral is carried out numerically. Computational results from UTD and physical optics (PO) analysis of a 34-m ground station dual-shaped reflector confirm the analytical formulations for both circularly symmetric and offset asymmetric subreflectors. It is concluded that the proposed PO(theta)GO(phi) technique can be used to study the spillover or noise temperature characteristics of a high-gain reflector antenna efficiently and accurately.

Evaluation of local anesthetic effects of Lidocaine-Ibuprofen ionic liquid stabilized silver nanoparticles in Male Swiss mice.

PubMed

Jiang, Qiliang; Yu, Shashuang; Li, Xingwang; Ma, Chuangen; Li, Aixiang

2018-01-01

A simple approach for the synthesis of Lidocaine-Ibuprofen ionic liquid stabilized silver nanoparticles (IL-AgNPs) was reported in this work. The shape, size and surface morphology of the Lidocaine-Ibuprofen ionic liquid stabilized AgNPs were characterized by using spectroscopic and microscopic techniques such as Ultraviolet-visible spectroscopy (UV-Visible), X-ray diffraction (XRD) analysis, Selected area electron diffraction (SAED), Transmission electron microscopy (TEM). TEM analysis showed the formation of 20-30nm size of IL-AgNPs with very clear lattice fringes. SAED pattern confirmed the highly crystalline nature of fabricated IL stabilized AgNPs. EDS results confirmed the formation of nanosilver. The fabricated IL-AgNPs were studied for their local anesthetic effect in rats. The results of local anesthetic effect showed that the time for onset of action by IL-AgNPs is 10min, which is significantly higher than that for EMLA. Further, tactile test results confirmed the stronger and faster local anesthetic effect of IL-AgNPs when compared to that of EMLA. Copyright © 2017. Published by Elsevier B.V.

Structural, optical and morphological studies of Cd2+ doping in CH3NH3PbI3 perovskite semiconductor at Pb2+ site for photovoltaic applications

NASA Astrophysics Data System (ADS)

Parrey, Khursheed; Warish, Mohd.; Devi, Nisha; Niazi, A.; Aziz, A.; Ansari, S. G.

2018-05-01

Doping of semiconductors in a controlled mannner have paramount technological importance as far as the optical and electronic properties of the devices are concerned. Hybrid organic-inorganic perovskites (HOPs) as intrinsic semiconductors have sensational properties required for both the solar photovoltaics and perovskite light emitting diodes. However, undoped and complexity in the dpoing process of HOPs have limited their exploitation in the field of elcronics. In this papper we present the synthesis of HOP semiconductor (CH3NH3PbI3) doped in Pb2+ position by Cd2+. We studied the effect of the incorporation of Cd2+ into the crystalline structure and analysed the changes in the properties like crystal structure, optical absorption and the surface morphology. The structure of HOPs confirmed by X-ray diffraction analysis is tetragonal perovskite type. It can be found that the crystallinity of the samples was enhanced with the doping concentration as the intensity of diffraction peaks were observed to increase with doping. The absorption spectra as obtained from UV-Visible spectrophotometry and Tauc plot analysis indicated that the band gap observed (1.73 eV) is direct type and gets reduced to 1.67 eV with the doping concentration. The red shift may be due to the increase in the size of nanocrystalline material with doping.

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

PubMed

Wang, Guangmei; Valldor, Martin; Spielberg, Eike T; Mudring, Anja-Verena

2014-03-17

A new framework cobalt(II) hydroxyl phosphate, Co2PO4OH, was prepared by ionothermal synthesis using 1-butyl-4-methyl-pyridinium hexafluorophosphate as the ionic liquid. As the formation of Co2PO4F competes in the synthesis, the synthesis conditions have to be judiciously chosen to obtain well-crystallized, single phase Co2PO4OH. Single-crystal X-ray diffraction analyses reveal Co2PO4OH crystallizes with space group I41/amd (a = b = 5.2713(7) Å, c = 12.907(3) Å, V = 358.63(10) Å(3), and Z = 4). Astonishingly, it does not crystallize isotypically with Co2PO4F but rather isotypically with the hydroxyl minerals caminite Mg1.33[SO4(OH)0.66(H2O)0.33] and lipscombite Fe(2–y)PO4(OH) (0 ≤ y ≤ 2/3). Phosphate tetrahedra groups interconnect four rod-packed face-sharing ∞(1){CoO(6/2)} octahedra chains to form a three-dimensional framework structure. The compound Co2PO4OH was further characterized by powder X-ray diffraction, Fourier transform–infrared, and ultraviolet–visible spectroscopy, confirming the discussed structure. The magnetic measurement reveals that Co2PO4OH undergoes a magnetic transition and presents at low temperatures a canted antiferromagnetic spin order in the ground state.

Controlled precipitation for enhanced dissolution rate of flurbiprofen: development of rapidly disintegrating tablets.

PubMed

Essa, Ebtessam A; Elmarakby, Amira O; Donia, Ahmed M A; El Maghraby, Gamal M

2017-09-01

The aim of this work was to investigate the potential of controlled precipitation of flurbiprofen on solid surface, in the presence or absence of hydrophilic polymers, as a tool for enhanced dissolution rate of the drug. The work was extended to develop rapidly disintegrated tablets. This strategy provides simple technique for dissolution enhancement of slowly dissolving drugs with high scaling up potential. Aerosil was dispersed in ethanolic solution of flurbiprofen in the presence and absence of hydrophilic polymers. Acidified water was added as antisolvent to produce controlled precipitation. The resultant particles were centrifuged and dried at ambient temperature before monitoring the dissolution pattern. The particles were also subjected to FTIR spectroscopic, X-ray diffraction and thermal analyses. The FTIR spectroscopy excluded any interaction between flurbiprofen and excipients. The thermal analysis reflected possible change in the crystalline structure and or crystal size of the drug after controlled precipitation in the presence of hydrophilic polymers. This was further confirmed by X-ray diffraction. The modulation in the crystalline structure and size was associated with a significant enhancement in the dissolution rate of flurbiprofen. Optimum formulations were successfully formulated as rapidly disintegrating tablet with subsequent fast dissolution. Precipitation on a large solid surface area is a promising strategy for enhanced dissolution rate with the presence of hydrophilic polymers during precipitation process improving the efficiency.

Effect of hydrogenation conditions on the microstructure and mechanical properties of zirconium hydride

NASA Astrophysics Data System (ADS)

Muta, Hiroaki; Nishikane, Ryoji; Ando, Yusuke; Matsunaga, Junji; Sakamoto, Kan; Harjo, Stefanus; Kawasaki, Takuro; Ohishi, Yuji; Kurosaki, Ken; Yamanaka, Shinsuke

2018-03-01

Precipitation of brittle zirconium hydrides deteriorate the fracture toughness of the fuel cladding tubes of light water reactor. Although the hydride embrittlement has been studied extensively, little is known about physical properties of the hydride due to the experimental difficulties. In the present study, to elucidate relationship between mechanical properties and microstructure, two δ-phase zirconium hydrides and one ε-phase zirconium hydride were carefully fabricated considering volume changes at the metal-to-hydride transformation. The δ-hydride that was fabricated from α-zirconium exhibits numerous inner cracks due to the large volume change. Analyses of the neutron diffraction pattern and electron backscatter diffraction (EBSD) data show that the sample displays significant stacking faults in the {111} plane and in the pseudo-layered microstructure. On the other hand, the δ-hydride sample fabricated from β-zirconium at a higher temperature displays equiaxed grains and no cracks. The strong crystal orientation dependence of mechanical properties were confirmed by indentation test and EBSD observation. The δ-hydride hydrogenated from α-zirconium displays a lower Young's modulus than that prepared from β-zirconium. The difference is attributed to stacking faults within the {111} plane, for which the Young's modulus exhibits the highest value in the perpendicular direction. The strong influence of the crystal orientation and dislocation density on the mechanical properties should be considered when evaluating hydride precipitates in nuclear fuel cladding.

Porphyrin framework solids. Synthesis and structure of hybrid coordination polymers of tetra(carboxyphenyl)porphyrins and lanthanide-bridging ions.

PubMed

Muniappan, Sankar; Lipstman, Sophia; George, Sumod; Goldberg, Israel

2007-07-09

New types of porphyrin-based framework solids were constructed by reacting meso-tetra(3-carboxyphenyl)porphyrin and meso-tetra(4-carboxyphenyl)metalloporphyrins with common salts of lanthanide metal ions. The large size, high coordination numbers and strong affinity for oxo ligands of the latter, combined with favorable hydrothermal reaction conditions, allowed the formation of open three-dimensional single-framework architectures by coordination polymerization, in which the tetradentate porphyrin units are intercoordinated by multinuclear assemblies of the bridging metal ions. The latter serve as construction pillars of the supramolecular arrays, affording stable structures. Several modes of coordination polymerization were revealed by single-crystal X-ray diffraction. They differ by the spatial functionality of the porphyrin building blocks, the coordination patterns of the lanthanide-carboxylate assemblies, and the topology of the resulting frameworks. The seven new reported structures exhibit periodically spaced 0.4-0.6 nm wide channel voids that perforate the respective crystalline polymeric architectures and are accessible to solvent components. Materials based on the m-carboxyphenyl derivative reveal smaller channels than those based on the p-carboxyphenyl analogues. An additional complex of the former with a smaller third-row transition metal (Co) is characterized by coordination connectivity in two dimensions only. Thermal and powder-diffraction analyses confirm the stability of the lanthanide-TmCPP (TmCPP=tetra(m-carboxyphenyl)porphyrin) frameworks.

Soy-based UV resistant polyurethane pultruded composites.

DOT National Transportation Integrated Search

2012-02-01

Aliphatic polyurethane (PU) nanocomposites were synthesized using organically modified nanoclays. X-Ray diffraction results : confirmed good exfoliation of nanoclay particles in the PU resin system. With the addition of just 1% of nanoclay in the bas...

Mineralogical and chemical characterization of iron-, manganese-, and copper-containing synthetic hydroxyapatites.

PubMed

Sutter, B; Ming, D W; Clearfield, A; Hossner, L R

2003-01-01

The National Aeronautics and Space Administration's (NASA) Advanced Life Support (ALS) Program is evaluating the use of Fe-, Mn-, and Cu-containing synthetic hydroxyapatite (SHA) as a slow release fertilizer for crops that might be grown on the International Space Station or at Lunar and Martian outposts. Separate Fe-, Mn-, and Cu-containing SHA materials along with a transition-metal free SHA (pure-SHA) were synthesized using a precipitation method. Chemical and mineralogical analyses determined if and how Fe, Mn, and Cu were incorporated into the SHA structure. X-ray diffraction (XRD), Rietveld refinement, and transmission electron microscopy (TEM) confirmed that SHA materials with the apatite structure were produced. Chemical analyses indicated that the metal containing SHA materials were deficient in Ca relative to pure-SHA. The shift in the infrared PO4-mu 3 vibrations, smaller unit cell parameters, smaller particle size, and greater structural strain for Fe-, Mn-, and Cu-containing SHA compared with pure-SHA suggested that Fe, Mn, and Cu were incorporated into SHA structure. Rietveld analyses revealed that Fe, Mn, and Cu substituted into the Ca2 site of SHA. An Fe-rich phase was detected by TEM analyses and backscattered electron microscopy in the Fe-containing SHA material with the greatest Fe content. The substitution of metals into SHA suggests that metal-SHA materials are potential slow-release sources of micronutrients for plant uptake in addition to Ca and P.

Mineralogical and chemical characterization of iron-, manganese-, and copper-containing synthetic hydroxyapatites

NASA Technical Reports Server (NTRS)

Sutter, B.; Ming, D. W.; Clearfield, A.; Hossner, L. R.

2003-01-01

The National Aeronautics and Space Administration's (NASA) Advanced Life Support (ALS) Program is evaluating the use of Fe-, Mn-, and Cu-containing synthetic hydroxyapatite (SHA) as a slow release fertilizer for crops that might be grown on the International Space Station or at Lunar and Martian outposts. Separate Fe-, Mn-, and Cu-containing SHA materials along with a transition-metal free SHA (pure-SHA) were synthesized using a precipitation method. Chemical and mineralogical analyses determined if and how Fe, Mn, and Cu were incorporated into the SHA structure. X-ray diffraction (XRD), Rietveld refinement, and transmission electron microscopy (TEM) confirmed that SHA materials with the apatite structure were produced. Chemical analyses indicated that the metal containing SHA materials were deficient in Ca relative to pure-SHA. The shift in the infrared PO4-mu 3 vibrations, smaller unit cell parameters, smaller particle size, and greater structural strain for Fe-, Mn-, and Cu-containing SHA compared with pure-SHA suggested that Fe, Mn, and Cu were incorporated into SHA structure. Rietveld analyses revealed that Fe, Mn, and Cu substituted into the Ca2 site of SHA. An Fe-rich phase was detected by TEM analyses and backscattered electron microscopy in the Fe-containing SHA material with the greatest Fe content. The substitution of metals into SHA suggests that metal-SHA materials are potential slow-release sources of micronutrients for plant uptake in addition to Ca and P.

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

PubMed

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

2012-03-01

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

Room temperature ferromagnetism of nanocrystalline Nd1.90Ni0.10O3-δ

NASA Astrophysics Data System (ADS)

Sarkar, B. J.; Mandal, J.; Dalal, M.; Bandyopadhyay, A.; Chakrabarti, P. K.

2018-05-01

Nanocrystalline sample of Ni2+ doped neodymium oxide (Nd1.90Ni0.10O3-δ, NNO) is synthesized by co-precipitation method. Analysis of X-ray diffraction (XRD) pattern by Rietveld refinement method confirms the desired phase of NNO and complete substitution of Ni2+ ions in the Nd2O3 lattice. Analyses of transmission electron microscopy (TEM) and Raman spectroscopy of NNO recorded at room temperature (RT) also substantiate this fact. Besides, no traces of impurities are found in the analyses of XRD, TEM and Raman data. Room temperature hysteresis loop of NNO suggests the presence of weak ferromagnetism (FM) in low field region ( 600 mT), but in high field region paramagnetism of the host is more prominent. Magnetization vs. temperature ( M- T) curve in the entire temperature range (300-5 K) is analyzed successfully by a combined equation generated from three-dimensional (3D) spin wave model and Curie-Weiss law, which suggests the presence of mixed paramagnetic phase together with ferromagnetic phase in the doped sample. The onset of magnetic ordering is analyzed by oxygen vacancy mediated F-center exchange (FCE) coupling mechanism.

Rocky 7 prototype Mars rover field geology experiments 1. Lavic Lake and sunshine volcanic field, California

USGS Publications Warehouse

Arvidson, R. E.; Acton, C.; Blaney, D.; Bowman, J.; Kim, S.; Klingelhofer, G.; Marshall, J.; Niebur, C.; Plescia, J.; Saunders, R.S.; Ulmer, C.T.

1998-01-01

Experiments with the Rocky 7 rover were performed in the Mojave Desert to better understand how to conduct rover-based, long-distance (kilometers) geological traverses on Mars. The rover was equipped with stereo imaging systems for remote sensing science and hazard avoidance and 57Fe Mo??ssbauer and nuclear magnetic resonance spectrometers for in situ determination of mineralogy of unprepared rock and soil surfaces. Laboratory data were also obtained using the spectrometers and an X ray diffraction (XRD)/XRF instrument for unprepared samples collected from the rover sites. Simulated orbital and descent image data assembled for the test sites were found to be critical for assessing the geologic setting, formulating hypotheses to be tested with rover observations, planning traverses, locating the rover, and providing a regional context for interpretation of rover-based observations. Analyses of remote sensing and in situ observations acquired by the rover confirmed inferences made from orbital and simulated descent images that the Sunshine Volcanic Field is composed of basalt flows. Rover data confirmed the idea that Lavic Lake is a recharge playa and that an alluvial fan composed of sediments with felsic compositions has prograded onto the playa. Rover-based discoveries include the inference that the basalt flows are mantled with aeolian sediment and covered with a dense pavement of varnished basalt cobbles. Results demonstrate that the combination of rover remote sensing and in situ analytical observations will significantly increase our understanding of Mars and provide key connecting links between orbital and descent data and analyses of returned samples. Copyright 1998 by the American Geophysical Union.

Detection of uranium and chemical state analysis of individual radioactive microparticles emitted from the Fukushima nuclear accident using multiple synchrotron radiation X-ray analyses.

PubMed

Abe, Yoshinari; Iizawa, Yushin; Terada, Yasuko; Adachi, Kouji; Igarashi, Yasuhito; Nakai, Izumi

2014-09-02

Synchrotron radiation (SR) X-ray microbeam analyses revealed the detailed chemical nature of radioactive aerosol microparticles emitted during the Fukushima Daiichi Nuclear Power Plant (FDNPP) accident, resulting in better understanding of what occurred in the plant during the early stages of the accident. Three spherical microparticles (∼2 μm, diameter) containing radioactive Cs were found in aerosol samples collected on March 14th and 15th, 2011, in Tsukuba, 172 km southwest of the FDNPP. SR-μ-X-ray fluorescence analysis detected the following 10 heavy elements in all three particles: Fe, Zn, Rb, Zr, Mo, Sn, Sb, Te, Cs, and Ba. In addition, U was found for the first time in two of the particles, further confirmed by U L-edge X-ray absorption near-edge structure (XANES) spectra, implying that U fuel and its fission products were contained in these particles along with radioactive Cs. These results strongly suggest that the FDNPP was damaged sufficiently to emit U fuel and fission products outside the containment vessel as aerosol particles. SR-μ-XANES spectra of Fe, Zn, Mo, and Sn K-edges for the individual particles revealed that they were present at high oxidation states, i.e., Fe(3+), Zn(2+), Mo(6+), and Sn(4+) in the glass matrix, confirmed by SR-μ-X-ray diffraction analysis. These radioactive materials in a glassy state may remain in the environment longer than those emitted as water-soluble radioactive Cs aerosol particles.

Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole

NASA Astrophysics Data System (ADS)

Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

2015-10-01

The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M = Mn(II), Fe(II) or Co(II); etim = 1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

Diffraction and forward physics results of the ATLAS experiment from the Run I

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

Taševský, Marek

Various aspects of forward physics have been studied by the ATLAS collaboration using data from Run I at the LHC. In this text, main results of four published analyses are summarized, all based on data from proton-proton collisions at √(s)=7 TeV collected in 2010 or 2011. Two analyses deal with the diffractive signature, one based on single-sided events, the other on large rapidity gaps in soft events. In addition, a recent measurement of the total pp cross section using the ALFA subdetector and a recent study of higher-order QCD effects using a jet veto are discussed.

Femtosecond time-resolved MeV electron diffraction

DOE PAGES

Zhu, Pengfei; Zhu, Y.; Hidaka, Y.; ...

2015-06-02

We report the experimental demonstration of femtosecond electron diffraction using high-brightness MeV electron beams. High-quality, single-shot electron diffraction patterns for both polycrystalline aluminum and single-crystal 1T-TaS 2 are obtained utilizing a 5 fC (~3 × 10 4 electrons) pulse of electrons at 2.8 MeV. The high quality of the electron diffraction patterns confirms that electron beam has a normalized emittance of ~50 nm rad. The transverse and longitudinal coherence length is ~11 and ~2.5 nm, respectively. The timing jitter between the pump laser and probe electron beam was found to be ~100 fs (rms). The temporal resolution is demonstrated bymore » observing the evolution of Bragg and superlattice peaks of 1T-TaS 2 following an 800 nm optical pump and was found to be 130 fs. Lastly, our results demonstrate the advantages of MeV electrons, including large elastic differential scattering cross-section and access to high-order reflections, and the feasibility of ultimately realizing below 10 fs time-resolved electron diffraction.« less

Excitation of surface waves on one-dimensional solid–fluid phononic crystals and the beam displacement effect

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

Moiseyenko, Rayisa P.; Georgia Institute of Technology, UMI Georgia Tech – CNRS, George W. Woodruff School of Mechanical Engineering, Georgia Tech Lorraine, 2 rue Marconi, 57070 Metz-Technopole; Liu, Jingfei

The possibility of surface wave generation by diffraction of pressure waves on deeply corrugated one-dimensional phononic crystal gratings is studied both theoretically and experimentally. Generation of leaky surface waves, indeed, is generally invoked in the explanation of the beam displacement effect that can be observed upon reflection on a shallow grating of an acoustic beam of finite width. True surface waves of the grating, however, have a dispersion that lies below the sound cone in water. They thus cannot satisfy the phase-matching condition for diffraction from plane waves of infinite extent incident from water. Diffraction measurements indicate that deeply corrugatedmore » one-dimensional phononic crystal gratings defined in a silicon wafer are very efficient diffraction gratings. They also confirm that all propagating waves detected in water follow the grating law. Numerical simulations however reveal that in the sub-diffraction regime, acoustic energy of a beam of finite extent can be transferred to elastic waves guided at the surface of the grating. Their leakage to the specular direction along the grating surface explains the apparent beam displacement effect.« less

IDATEN and G-SITENNO: GUI-assisted software for coherent X-ray diffraction imaging experiments and data analyses at SACLA.

PubMed

Sekiguchi, Yuki; Yamamoto, Masaki; Oroguchi, Tomotaka; Takayama, Yuki; Suzuki, Shigeyuki; Nakasako, Masayoshi

2014-11-01

Using our custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors, cryogenic coherent X-ray diffraction imaging experiments have been undertaken at the SPring-8 Angstrom Compact free electron LAser (SACLA) facility. To efficiently perform experiments and data processing, two software suites with user-friendly graphical user interfaces have been developed. The first is a program suite named IDATEN, which was developed to easily conduct four procedures during experiments: aligning KOTOBUKI-1, loading a flash-cooled sample into the cryogenic goniometer stage inside the vacuum chamber of KOTOBUKI-1, adjusting the sample position with respect to the X-ray beam using a pair of telescopes, and collecting diffraction data by raster scanning the sample with X-ray pulses. Named G-SITENNO, the other suite is an automated version of the original SITENNO suite, which was designed for processing diffraction data. These user-friendly software suites are now indispensable for collecting a large number of diffraction patterns and for processing the diffraction patterns immediately after collecting data within a limited beam time.

Amorphous Phase Characterization Through X-Ray Diffraction Profile Modeling: Implications for Amorphous Phases in Gale Crater Rocks and Soils

NASA Technical Reports Server (NTRS)

Achilles, C. N.; Downs, G. W.; Downs, R. T.; Morris, R. V.; Rampe, E. B.; Ming, D. W.; Chipera, S. J.; Blake, D. F.; Vaniman, D. T.; Bristow, T. F.;

Total-scattering pair-distribution function of organic material from powder electron diffraction data

DOE PAGES

Gorelik, Tatiana E.; Billinge, Simon J. L.; Schmidt, Martin U.; ...

2015-04-01

This paper shows for the first time that pair-distribution function analyses can be carried out on organic and organo-metallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction (SAED) and nanodiffraction in transmission electron microscopy (TEM) or nanodiffraction in scanning transmission electron microscopy (STEM) modes. The methods were demonstrated on organo-metallic complexes (chlorinated and unchlorinated copper-phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering datamore » and avoiding beam-damage of the sample are possible to resolve.« less

Insights on the origin of the Tb5Ge4 magnetocaloric effect

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

Belo, J. H.; Barbosa, M. B.; Pires, A. L.

2017-05-01

In this report the magnetic, atomic structures and spin-lattice coupling have been thoroughly studied through high magnetic field magnetometry, Synchrotron X-ray diffraction under applied magnetic field and magnetostriction measurements in the Tb5Ge4 compounds. A field induced phase transition from an antiferromagnetic towards a ferromagnetic ordering was confirmed but with absence of structural transformation. This absence has been confirmed experimentally through synchrotron x-ray diffraction under applied field (up to 30 T). Moreover, this absence was explained via a thermodynamic free energy model: first principles calculations determined a large energy gap (ΔE=0.65 eV) between the two possible structures, O(I) and O(II). Frommore » magnetic and structural properties, a H-T phase diagram has been proposed for Tb5Ge4. Finally it was observed a large magnetostriction (up to 600 ppm) induced by ΔH=7 T.« less

Alternative approaches used to assess structural changes of natural zircon caused by heat treatment

NASA Astrophysics Data System (ADS)

Huong, L. T. T.; Thuyet, N. T. M.; Phan, T. L.; Tran, N.; Toan, D. N.; Thang, P. D.; Huy, B. T.

2018-03-01

It is known that large changes in the crystal structure of zircon (ZrSiO4) can be assessed through the linewidth of the characteristic Raman mode (Δν3) at 1008 cm-1. However, the use of Δν3 to assess small changes caused by heat treatment at temperatures below its decomposition temperature of 1670 °C is difficult. The present work points out that the combination of X-ray diffraction (XRD) analyses, and photoluminescence (PL) and Raman (RS) measurements with different excitation wavelengths is an effective approach to solve the above problem. In this context, we have selected natural zircon containing some rare-earth (RE) impurities, and then studied the changes in its crystal structure caused by heat treatment at temperatures Tan=400-1600 °C. XRD analyses reveal that small modifications of the unit-cell parameters occur as Tan>600 °C. Taking the intensity ratios of the ν3 mode to RE-related emissions (Iν3/IRE) or the PL intensity ratios between RE-related emissions into consideration, the similar results in good agreement with the XRD analyses are also found. We believe that the small structural changes are related to the migration and redistribution of defects and impurities, and re-crystallization of zircon. This could be further confirmed though the relation between paramagnetic and ferromagnetic signals when Tan changes.

Characterisation of silica derived from rice husk (Muar, Johor, Malaysia) decomposition at different temperatures

NASA Astrophysics Data System (ADS)

Azmi, M. A.; Ismail, N. A. A.; Rizamarhaiza, M.; W. M. Hasif. A. A., K.; Taib, H.

2016-07-01

Rice husk was thermally decomposed to yield powder composed of silica (SiO2). Temperatures of 700°C and 1000°C were chosen as the decomposition temperatures. X-Ray Diffraction (XRD), X-Ray Florescence (XRF), Fourier Transform Infrared (FTIR), and Field Emission Scanning Electron Microscope (FESEM) analyses were conducted on a synthetic silica powder (SS-SiO2) and the rice husk ash as for the comparative characterisation study. XRD analyses clearly indicated that the decomposed rice husk yielded silica of different nature which are Crystalline Rice Husk Silica (C-RHSiO2) and Amorphous Rice Husk Silica (A-RHSiO2). Moreover, it was found that SS-SiO2 was of Quartz phase, C-RHSiO2 was of Trydimite and Cristobalite. Through XRF detection, the highest SiO2 purity was detected in SS-SiO2 followed by C-RHSiO2 and A-RHSiO2 with purity percentages of 99.60%, 82.30% and 86.30% respectively. FTIR results clearly indicated silica (SiO2) bonding 1056, 1064, 1047, 777, 790 and 798 cm-1) increased as the crystallinity silica increased. The Cristobalite phase was detected in C-RH SiO2 at the wavelength of 620 cm-1. Morphological features as observed by FESEM analyses confirmed that, SS-SiO2 and C-RH SiO2 showed prominent coarse granular morphology.

Advanced setup for high-pressure and low-temperature neutron diffraction at hydrostatic conditions

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

Lokshin, Konstantin A.; Zhao Yusheng

2005-06-15

We describe a design of the experimental setup for neutron diffraction studies at low temperatures and hydrostatic pressure. The significant benefit of the setup, compared to the previous methods, is that it makes possible the simultaneous collection of neutrons diffracted at the 30 deg. -150 deg. range with no contamination by the primary scattering from the sample surroundings and without cutting out the incident and diffracted beams. The suggested design is most useful for third-generation time-of-flight diffractometers and constant wavelength instruments. Application of the setup expands the capabilities of high-pressure neutron diffraction, allowing time-resolved kinetics and structural studies, multihistogram Rietveld,more » and pair distribution function and texture analyses. The high efficiency of the setup was proven for the HIPPO diffractometer at Los Alamos Neutron Science Center under pressures up to 10 kbar and temperatures from 4 to 300 K.« less

Statistical Limits to Super Resolution

NASA Astrophysics Data System (ADS)

Lucy, L. B.

1992-08-01

The limits imposed by photon statistics on the degree to which Rayleigh's resolution limit for diffraction-limited images can be surpassed by applying image restoration techniques are investigated. An approximate statistical theory is given for the number of detected photons required in the image of an unresolved pair of equal point sources in order that its information content allows in principle resolution by restoration. This theory is confirmed by numerical restoration experiments on synthetic images, and quantitative limits are presented for restoration of diffraction-limited images formed by slit and circular apertures.

Investigation of experimental pole-figure errors by simulation of individual spectra

NASA Astrophysics Data System (ADS)

Lychagina, T. A.; Nikolaev, D. I.

2007-09-01

The errors in measuring the crystallographic texture described by pole figures are studied. A set of diffraction spectra for a sample of the MA2-1 alloy (Mg + 4.5% Al + 1% Zn) are measured, simulation of individual spectra on the basis of which the pole figures were obtained is performed, and their errors are determined. The conclusion about the possibility of determining the effect of errors of the diffraction peak half-width on the pole figure errors that was drawn in our previous studies is confirmed.

Biosynthesis of silver nanoparticles using fresh extracts of Tridax procumbens linn.

PubMed

Bhati-Kushwaha, Himakshi

2014-04-01

A simple and eco-friendly method for the synthesis of biogenic nanoparticles (NP's) using an aqueous solution of T. procumbens fresh plant extract (leaf and stem) as a bioreductant is reported. The prepared biogenic nanoparticles were well characterized using U.V. visible spectroscopy, scanning electron microscopy, X-ray diffraction and Fourier-transform infrared spectroscopy. The particles were confirmed to be elemental crystal by X-ray diffraction. The potential applications of biosynthesized nanoparticles as antimicrobial (antibacterial and antifungal) against pathogens Escherichia coli, Vibrio cholerae, Aspergillus niger and Aspergillusflavus were demonstrated.

Energy Dispersive X-ray Diffraction (EDXRD) of Li1.1V3O8 Electrochemical Cell

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

Zhang, Qing; Bruck, Andrea M.; Bock, David C.

2017-01-01

ABSTRACT In this study, we conducted the first energy dispersive x-ray diffraction (EDXRD) experiments on Li/Li 1.1V 3O 8coin cells discharged to different lithiation levels in order to investigate the phase transitions upon electrochemical reduction. The phase transformation from layered Li-poor α to Li-rich α to defect rock-salt β phase was confirmed with cells of different lithiation stages. No spatial localization of phase formation was observed throughout the cathodes under the conditions of this measurement.

Energy Dispersive X-ray Diffraction (EDXRD) of Li1.1V3O8 Electrochemical Cell

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

Zhang, Qing; Bruck, Andrea M.; Bock, David C.

ABSTRACT In this study, we conducted the first energy dispersive x-ray diffraction (EDXRD) experiments on Li/Li 1.1V 3O 8coin cells discharged to different lithiation levels in order to investigate the phase transitions upon electrochemical reduction. The phase transformation from layered Li-poor α to Li-rich α to defect rock-salt β phase was confirmed with cells of different lithiation stages. No spatial localization of phase formation was observed throughout the cathodes under the conditions of this measurement.

Readout signals calculated for near-field optical pickups with land and groove recording.

PubMed

Saito, K; Kishima, K; Ichimura, I

2000-08-10

Optical disk readout signals with a solid immersion lens (SIL) and the land-groove recording technique are calculated by use of a simplified vector-diffraction theory. In this method the full vector-diffraction theory is applied to calculate the diffracted light from the initial state of the disk, and the light scattered from the recorded marks is regarded as a perturbation. Using this method, we confirmed that the land-groove recording technique is effective as a means of cross-talk reduction even when the numerical aperture is more than 1. However, the top surface of the disk under the SIL must be flat, or the readout signal from marks recorded on a groove decays when the optical depth of the groove is greater than lambda/8.

Accuracy in Rietveld quantitative phase analysis: a comparative study of strictly monochromatic Mo and Cu radiations.

PubMed

León-Reina, L; García-Maté, M; Álvarez-Pinazo, G; Santacruz, I; Vallcorba, O; De la Torre, A G; Aranda, M A G

2016-06-01

This study reports 78 Rietveld quantitative phase analyses using Cu  K α 1 , Mo  K α 1 and synchrotron radiations. Synchrotron powder diffraction has been used to validate the most challenging analyses. From the results for three series with increasing contents of an analyte (an inorganic crystalline phase, an organic crystalline phase and a glass), it is inferred that Rietveld analyses from high-energy Mo  K α 1 radiation have slightly better accuracies than those obtained from Cu  K α 1 radiation. This behaviour has been established from the results of the calibration graphics obtained through the spiking method and also from Kullback-Leibler distance statistic studies. This outcome is explained, in spite of the lower diffraction power for Mo radiation when compared to Cu radiation, as arising because of the larger volume tested with Mo and also because higher energy allows one to record patterns with fewer systematic errors. The limit of detection (LoD) and limit of quantification (LoQ) have also been established for the studied series. For similar recording times, the LoDs in Cu patterns, ∼0.2 wt%, are slightly lower than those derived from Mo patterns, ∼0.3 wt%. The LoQ for a well crystallized inorganic phase using laboratory powder diffraction was established to be close to 0.10 wt% in stable fits with good precision. However, the accuracy of these analyses was poor with relative errors near to 100%. Only contents higher than 1.0 wt% yielded analyses with relative errors lower than 20%.

Application of δ recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes.

PubMed

Rius, Jordi; Mugnaioli, Enrico; Vallcorba, Oriol; Kolb, Ute

2013-07-01

δ Recycling is a simple procedure for directly extracting phase information from Patterson-type functions [Rius (2012). Acta Cryst. A68, 399-400]. This new phasing method has a clear theoretical basis and was developed with ideal single-crystal X-ray diffraction data. On the other hand, introduction of the automated diffraction tomography (ADT) technique has represented a significant advance in electron diffraction data collection [Kolb et al. (2007). Ultramicroscopy, 107, 507-513]. When combined with precession electron diffraction, it delivers quasi-kinematical intensity data even for complex inorganic compounds, so that single-crystal diffraction data of nanometric volumes are now available for structure determination by direct methods. To check the tolerance of δ recycling to missing data-collection corrections and to deviations from kinematical behaviour of ADT intensities, δ recycling has been applied to differently shaped nanocrystals of various inorganic materials. The results confirm that it can phase ADT data very efficiently. In some cases even more complete structure models than those derived from conventional direct methods and least-squares refinement have been found. During this study it has been demonstrated that the Wilson-plot scaling procedure is largely insensitive to sample thickness variations and missing absorption corrections affecting electron ADT intensities.

Toward in situ x-ray diffraction imaging at the nanometer scale

NASA Astrophysics Data System (ADS)

Zatsepin, Nadia A.; Dilanian, Ruben A.; Nikulin, Andrei Y.; Gable, Brian M.; Muddle, Barry C.; Sakata, Osami

2008-08-01

We present the results of preliminary investigations determining the sensitivity and applicability of a novel x-ray diffraction based nanoscale imaging technique, including simulations and experiments. The ultimate aim of this nascent technique is non-destructive, bulk-material characterization on the nanometer scale, involving three dimensional image reconstructions of embedded nanoparticles and in situ sample characterization. The approach is insensitive to x-ray coherence, making it applicable to synchrotron and laboratory hard x-ray sources, opening the possibility of unprecedented nanometer resolution with the latter. The technique is being developed with a focus on analyzing a technologically important light metal alloy, Al-xCu (where x is 2.0-5.0 %wt). The mono- and polycrystalline samples contain crystallographically oriented, weakly diffracting Al2Cu nanoprecipitates in a sparse, spatially random dispersion within the Al matrix. By employing a triple-axis diffractometer in the non-dispersive setup we collected two-dimensional reciprocal space maps of synchrotron x-rays diffracted from the Al2Cu nanoparticles. The intensity profiles of the diffraction peaks confirmed the sensitivity of the technique to the presence and orientation of the nanoparticles. This is a fundamental step towards in situ observation of such extremely sparse, weakly diffracting nanoprecipitates embedded in light metal alloys at early stages of their growth.

Development of carboxymethyl cellulose-based hydrogel and nanosilver composite as antimicrobial agents for UTI pathogens.

PubMed

Alshehri, Saad M; Aldalbahi, Ali; Al-Hajji, Abdullah Baker; Chaudhary, Anis Ahmad; Panhuis, Marc In Het; Alhokbany, Norah; Ahamad, Tansir

2016-03-15

Silver nanoparticles (AgNPs) containing hydrogel composite were first synthesized by preparing a new hydrogel from carboxymethyl cellulose (CMC), polyvinyl alcohol (PVA), and the cross-linker ethylene glycol diglycidyl ether (EGDE), followed by the incorporation of AgNPs by microwave radiation. The resulting neat hydrogels and AgNPs-hydrogel composites were characterized using spectral, thermal, microscopic analysis and X-ray diffraction (XRD) analyses. The SEM and TEM results demonstrated that the synthesized AgNPs were spherical with diameters ranging from 8 to 14nm. In addition, the XRD analysis confirmed the nanocrystalline phase of silver with face-centered cubic (FCC) crystal structure. Energy dispersive spectroscopy (EDS) analysis of the AgNPs confirmed the presence of an elemental silver signal, and no peaks of any other impurities were detected. Additionally, the antibacterial activities of the neat hydrogel and AgNPs-hydrogel composites were measured by Kirby-Bauer method against urinary tract infection (UTI) pathogens. The rheology measurement revealed that the values of storage modulus (G') were higher than that of loss modulus (G″). The AgNPs-hydrogel composites exhibited higher antibacterial activity against Escherichia coli, Klebsiella pneumoniae, Pseudomonas aeruginosa, Proteus vulgaris, Staphylococcus aureus and Proteus mirabilis compared to the corresponding neat hydrogel. Copyright © 2015 Elsevier Ltd. All rights reserved.

Structural, morphological and gas sensing study of zinc doped tin oxide nanoparticles synthesized via hydrothermal technique

NASA Astrophysics Data System (ADS)

Singh, Davender; Kundu, Virender Singh; Maan, A. S.

2016-07-01

The pure and Zn-doped SnO2 nanoparticles were prepared successfully by hydrothermal route on large scale having different doping concentration of zinc from 0 to 0.20%. The calcined nanoparticles were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM) for structural and morphological studies. XRD analyses reveal that the nanoparticles of these doping concentrations are polycrystalline in nature and existed as tetragonal rutile structure, SEM study of images confirms the existence of very small, homogeneously distributed, and spherical nanoparticles. The particles size of the nanoparticles was calculated by Scherrer formula and was found in the range of 9-21 nm. The presence of dopant (i.e. zinc) and formation of Sn-O phase and hydrous nature of Zn-doped SnO2 nanoparticles are confirmed by EDX and FTIR study. The gas sensing properties of pure and Zn-doped SnO2 nanoparticles were investigated for various concentrations of methanol, ethanol and acetone at different operating temperatures and it has been found that with doping concentration of zinc (x = 0.20%) shows the maximum response 78% to methanol, 65% to ethanol and 62% to acetone respectively at different operating temperature within the measurement limit for a concentration of 100 ppm of each gases.

Effect of the nanosized TiO2 particles in Pd/C catalysts as cathode materials in direct methanol fuel cells.

PubMed

Choi, Mahnsoo; Han, Choonsoo; Kim, In-Tae; Lee, Ji-Jung; Lee, Hong-Ki; Shim, Joongpyo

2011-07-01

Pd-TiO2/C catalysts were prepared by impregnating titanium dioxide (TiO2) on carbon-supported Pd (Pd/C) for use as the catalyst for the oxygen reduction reaction (ORR) in direct methanol fuel cells (DMFCs). Transmission electron microscope (TEM), scanning electron microscope (SEM) and X-ray diffraction (XRD) analyses were carried to confirm the distribution, morphology and structure of Pd and TiO2 on the carbon support. In fuel cell test, we confirmed that the addition of TiO2 nanoparticles make the improved catalytic activity of oxygen reduction. The electrochemical characterization of the Pd-TiO2/C catalyst for the ORR was carried out by cyclic voltammetry (CV) in the voltage window of 0.04 V to 1.2 V with scan rate of 25 mV/s. With the increase in the crystallite size of TiO2, the peak potential for OH(ads) desorption on the surface of Pd particle shifted to higher potential. This implies that TiO2 might affect the adsorption and desorption of oxygen molecules on Pd catalyst. The performance of Pd-TiO2/C as a cathode material was found to be similar to or better performance than that of Pt/C.

Structural and photocatalytic studies of hydrothermally synthesized Mn2+-TiO2 nanoparticles under UV and visible light irradiation

NASA Astrophysics Data System (ADS)

Kamble, Ravi; Sabale, Sandip; Chikode, Prashant; Puri, Vijaya; Mahajan, Smita

2016-11-01

Pure TiO2 and Mn2+-TiO2 nanoparticles have been prepared by simple hydrothermal method with different Mn2+ concentrations. Obtained samples were analysed to determine it’s structural, optical, morphological and compositional properties using x-ray diffraction, UV-DRS, Raman, photoluminescence, XPS, TEM and EDS analysis. The EDS micrograph confirms the existence of Mn2+ atoms in TiO2 matrix with 0.86, 1.60 and 1.90 wt%. The crystallite size as well as band gap decreases with increase in Mn2+ concentration. The average particle size obtained from TEM was found 8-11 nm which is in good agreement with XRD results. Raman bands at 640, 518 and 398 cm-1 further confirmed pure phase anatase in all samples. XPS shows the proper substitutions of few sites of Ti4+ ions by Mn2+ ions in the TiO2 host lattice. The intensity of PL spectra for Mn2+-TiO2 shows a gradual decrease in the peak intensity with increasing Mn2+ concentration in TiO2, it implies lower electron-hole recombination rate as Mn2+ ions increases. The obtained samples were further studied for its photocatalytic activities using malachite green dye under UV light and visible light.

Epitaxial growth of mixed conducting layered Ruddlesden–Popper La{sub n+1}Ni{sub n}O{sub 3n+1} (n = 1, 2 and 3) phases by pulsed laser deposition

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

Wu, Kuan-Ting; Soh, Yeong-Ah; Skinner, Stephen J., E-mail: s.skinner@imperial.ac.uk

2013-10-15

Graphical abstract: - Highlights: • High quality epitaxial thin films of layered Ruddlesden–Popper nickelates were prepared. • For the first time this has been achieved by the PLD process. • n = 1, 2 and 3 films were successfully deposited on SrTiO{sub 3} and NdGaO{sub 3} substrates. • c-Axis oriented films were confirmed by XRD analysis. • In-plane and out-of-plane strain effects on lattice are discussed. - Abstract: Layered Ruddlesden–Popper phases of composition La{sub n+1}Ni{sub n}O{sub 3n+1} (n = 1, 2 and 3) have been epitaxially grown on SrTiO{sub 3} (0 0 1) or NdGaO{sub 3} (1 1 0) singlemore » crystal substrates using the pulsed laser deposition technique. X-ray diffraction analyses (θ/2θ, rocking curves, and φ-scans) and atomic force microscopy confirms the high-quality growth of the series of films with low surface roughness values (less than 1 nm). In particular, epitaxial growth of the higher order phases (n = 2 and 3) of lanthanum nickelate have been demonstrated for the first time.« less

Physicochemical characterization of novel Schiff bases derived from developed bacterial cellulose 2,3-dialdehyde.

PubMed

Keshk, Sherif M A S; Ramadan, Ahmed M; Bondock, Samir

2015-08-20

The synthesis of two novel Schiff's bases (cellulose-2,3-bis-[(4-methylene-amino)-benzene-sulfonamide] (5) & cellulose-2,3-bis-[(4-methylene-amino)-N-(thiazol-2-yl)-benzenesulfonamide] (6) via condensation reactions of periodate oxidized developed bacterial cellulose ODBC (2) with sulfa drugs [sulfanilamide (3) & sulfathiazole (4)] was reported. The physicochemical characterization of the condensation products was performed using FTIR, (1)H NMR, (13)C NMR spectral analyses, X-ray diffraction and DTA. The ODBC exhibited the highest degree of oxidation based on the aldehyde group number percentage (82.9%), which confirms the highest reactivity of developed bacterial cellulose [DBC (1)]. The X-ray diffractograms indicated an increase in the interplanar distance of the cellulose Schiff base (6) compared to ODBC (2) due to sulfathiazole (4) inclusion between ODBC (2) sheets corresponding to the 1 1 0 plane. In addition, the aldehyde content of Schiff base (6) was (20.8%) much lower than that of Schiff base (5) (41.5%). These results confirmed the high affinity of sulfathiazole (4) to the ODBC (2) chain, and the substantial changes in the original properties of ODBC were due to these chemical modifications rather than the sulfanilamide (3). Copyright © 2015 Elsevier Ltd. All rights reserved.

Electrochemical reduction behavior of simplified simulants of vitrified radioactive waste in molten CaCl2

NASA Astrophysics Data System (ADS)

Katasho, Yumi; Yasuda, Kouji; Nohira, Toshiyuki

2018-05-01

The electrochemical reduction of two types of simplified simulants of vitrified radioactive waste, simulant 1 (glass component only: SiO2, B2O3, Na2O, Al2O3, CaO, Li2O, and ZnO) and simulant 2 (also containing long-lived fission product oxides, ZrO2, Cs2O, PdO, and SeO2), was investigated in molten CaCl2 at 1103 K. The behavior of each element was predicted from the potential-pO2- diagram constructed from thermodynamic data. After the immersion of simulant 1 into molten CaCl2 without electrolysis, the dissolution of Na, Li, and Cs was confirmed by inductively coupled plasma atomic emission spectrometry and mass spectrometry analysis of the samples. The scanning electron microscopy/energy dispersive X-ray and X-ray diffraction analyses of simulants 1 and 2 electrolyzed at 0.9 V vs. Ca2+/Ca confirmed that most of SiO2 had been reduced to Si. After the electrolysis of simulants 1 and 2, Al, Zr, and Pd remained in the solid phase. In addition, SeO2 was found to remain partially in the solid phase and partially evaporate, although a small quantity dissolved into the molten salt.

Synthesis of AuPd alloyed nanoparticles via room-temperature electron reduction with argon glow discharge as electron source.

PubMed

Yang, Manman; Wang, Zongyuan; Wang, Wei; Liu, Chang-Jun

2014-01-01

Argon glow discharge has been employed as a cheap, environmentally friendly, and convenient electron source for simultaneous reduction of HAuCl4 and PdCl2 on the anodic aluminum oxide (AAO) substrate. The thermal imaging confirms that the synthesis is operated at room temperature. The reduction is conducted with a short time (30 min) under the pressure of approximately 100 Pa. This room-temperature electron reduction operates in a dry way and requires neither hydrogen nor extra heating nor chemical reducing agent. The analyses using X-ray photoelectron spectroscopy (XPS) confirm all the metallic ions have been reduced. The characterization with X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) shows that AuPd alloyed nanoparticles are formed. There also exist some highly dispersed Au and Pd monometallic particles that cannot be detected by XRD and transmission electron microscopy (TEM) because of their small particle sizes. The observed AuPd alloyed nanoparticles are spherical with an average size of 14 nm. No core-shell structure can be observed. The room-temperature electron reduction can be operated in a larger scale. It is an easy way for the synthesis of AuPd alloyed nanoparticles.

Perovskite-Type Oxides. I. Structural, Magnetic, and Morphological Properties of LaMn 1- xCu xO 3 and LaCo 1- xCu xO 3 Solid Solutions with Large Surface Area

NASA Astrophysics Data System (ADS)

Porta, Piero; De Rossi, Sergio; Faticanti, Marco; Minelli, Giuliano; Pettiti, Ida; Lisi, Luciana; Turco, Maria

1999-09-01

Perovskite-type compounds of general formula LaMn1-xCuxO3 and LaCo1-xCuxO3 (x=0.0, 0.2, 0.4, 0.6, 0.8, 1.0) were prepared by calcining the citrate gel precursors at 823, 923, and 1073 K. The decomposition of the precursors was followed by thermal analysis and the oxides were investigated by means of elemental analysis (atomic absorption and redox titration), X-ray powder diffraction, BET surface area, X-ray absorption (EXAFS and XANES), electron microscopy (SEM and TEM), and magnetic susceptibility. LaMn1-xCuxO3 samples are perovskite-like single phases up to x=0.6. At x=0.8 CuO and La2CuO4 phases are present in addition to perovskite. For x=1.0 the material is formed by CuO and La2CuO4. Mn(IV) was found by redox titration in all Mn-based perovskite samples, its fraction increasing with the increase in copper content. EXAFS and XANES analyses confirmed the presence of Mn(IV). Cation vacancies in equal amounts in the 12-coordinated A and octahedral B sites are suggested in the samples with x=0.0 and x=0.2, while for x=0.6 anionic vacancies are present. Materials with sufficiently high surface area (22-36 m2 g-1 for samples fired at 923 K and 14-22 m2 g-1 for those fired at 1073 K) were obtained. Crystallite sizes in the ranges 390-500 and 590-940 Å for samples calcined at 923 and 1073 K, respectively, were determined from the FWHM of the (102) X-ray diffraction peak. TEM patterns of LaMnO3 showed almost regular hexagonal prismatic crystals with sizes of the same order of magnitude (800 Å) of those drawn from X-ray diffraction, while no evidence of defect clustering was drawn out from TEM and electron diffraction images. For the sample with x=0.6, TEM and electron diffraction patterns revealed perturbation of the structure. Magnetic susceptibility studies show a ferromagnetic behavior that decreases with increase in x. LaCo1-xCuxO3 samples are perovskite-like single phases up to x=0.2. For x=0.4 a small amount of La2CuO4, in addition to perovskite, is detected. For x≥0.6 massive formation of La2CuO4 and CuO is observed. Only trivalent cobalt is found by redox titration. Magnetic susceptibility studies have shown that trivalent cobalt is present in all samples as a mixture of paramagnetic Co3+ and diamagnetic CoIII ions, the Co3+ fraction being, at least up to x=0.4, equal to ≈0.34. Antiferromagnetic behavior, which increases with increase in x, is observed in all LaCo1-xCuxO3 samples. LaCoO3 is a stoichiometric perovskite. The substitution of cobalt by Cu2+ leads to a positive charge defectivity which is compensated by oxygen vacancies. EXAFS and XANES analyses confirmed the presence of trivalent cobalt. Materials with fairly high surface area (in the ranges 19-27 and 13-21 m2 g-1 for samples calcined at 923 and 1073 K, respectively) were obtained. Crystallite sizes of ≈400 and ≈1000 Å for samples calcined at 923 and 1073 K, respectively, were determined from the FWHM of the (102) X-ray diffraction peak. Materials with not very clear morphology and crystals with definite structure are distinguishable by SEM for samples calcined at 1073 and at 1273 K, respectively. TEM patterns, for samples calcined at 1073 K, evidence almost regular hexagonal prismatic crystals connected to form "linked structures" and some "spotty crystals," suggesting short-range ordered local defects. For copper-containing samples, calcined at 1273 K, a higher degree of defectivity (probably associated with the interaction of anion vacancies) and the occurrence of "planar faults" are shown by TEM.

Structural, dielectric and impedance studies of polycrystalline La0.6Dy0.2Ca0.2MnO3

NASA Astrophysics Data System (ADS)

Nandan, K. R.; Kumar, A. Ruban

2017-05-01

Polycrystalline materials of Dy doped La1-xCaxMnO3 were prepared by Sol-Gel technique using citric acid as a chelating agent at 900°C. The compound was analyzed by powder X-ray diffraction technique and confirmed to be single phased orthorhombic perovskite structure with space group Pnma. From the dielectric and impedance studies confirmed the existence of dielectric relaxation and presence of space charge were observed from the dielectric constant and impedance plots respectively and confirms the existence of relaxation due to oxygen vacancy. Cole-cole plot confirms the presence of dielectric relaxation and grain contribution in the synthesized sample.

Dark-field phase retrieval under the constraint of the Friedel symmetry in coherent X-ray diffraction imaging.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Nakasako, Masayoshi

2014-11-17

Coherent X-ray diffraction imaging (CXDI) is a lensless imaging technique that is suitable for visualizing the structures of non-crystalline particles with micrometer to sub-micrometer dimensions from material science and biology. One of the difficulties inherent to CXDI structural analyses is the reconstruction of electron density maps of specimen particles from diffraction patterns because saturated detector pixels and a beam stopper result in missing data in small-angle regions. To overcome this difficulty, the dark-field phase-retrieval (DFPR) method has been proposed. The DFPR method reconstructs electron density maps from diffraction data, which are modified by multiplying Gaussian masks with an observed diffraction pattern in the high-angle regions. In this paper, we incorporated Friedel centrosymmetry for diffraction patterns into the DFPR method to provide a constraint for the phase-retrieval calculation. A set of model simulations demonstrated that this constraint dramatically improved the probability of reconstructing correct electron density maps from diffraction patterns that were missing data in the small-angle region. In addition, the DFPR method with the constraint was applied successfully to experimentally obtained diffraction patterns with significant quantities of missing data. We also discuss this method's limitations with respect to the level of Poisson noise in X-ray detection.

Investigation on the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ manganites

NASA Astrophysics Data System (ADS)

Arun, B.; Athira, M.; Akshay, V. R.; Sudakshina, B.; Mutta, Geeta R.; Vasundhara, M.

2018-02-01

We have investigated the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ Perovskite manganites. Rietveld refinement of the X-ray powder diffraction patterns confirms that all the studied compounds have crystallized into an orthorhombic structure with Pbnm space group. Transmission electron microscopy analysis reveals nanocrystalline compounds with crystallite size less than 50 nm. The selected area electron diffraction patterns reveal the highly crystalline nature of the compounds and energy dispersive X-ray spectroscopic analysis shows that the obtained compositions are nearly identical with the nominal one. The oxygen stoichiometry is estimated by iodometric titration method and stoichiometric compositions are confirmed by X-ray Fluorescence Spectrometry analysis. A large bifurcation is observed in the ZFC/FC curves and Arrott plots not show a linear relation but have a convex curvature nature. The temperature dependence of inverse magnetic susceptibility at higher temperature confirms the existence of ferromagnetic clusters. The experimental results reveal that the reduction of crystallite size to nano metric scale in Pr-deficient manganites adversely influences structural, magnetic and magnetocaloric properties as compared to its bulk counterparts reported earlier.

Spectroscopic and x-ray diffraction analyses of asbestos in the World Trade Center dust:

USGS Publications Warehouse

Swayze, Gregg A.; Clark, Roger N.; Sutley, Stephen J.; Hoefen, Todd M.; Plumlee, Geoffrey S.; Meeker, Gregory P.; Brownfield, Isabelle; Livo, Keith E.; Morath, Laurie C.

2009-01-01

On September 17 and 18, 2001, samples of settled dust and airfall debris were collected from 34 sites within a 1-km radius of the WTC collapse site, including a sample from an indoor location unaffected by rainfall, and samples of insulation from two steel beams at Ground Zero. Laboratory spectral and x-ray diffraction analyses of the field samples detected trace levels of serpentine minerals, including chrysotile asbestos, in about two-thirds of the dust samples at concentrations at or below ~1 wt%. One sample of a beam coating material contained up to 20 wt% chrysotile asbestos. Analyses indicate that trace levels of chrysotile were distributed with the dust radially to distances greater than 0.75 km from Ground Zero. The chrysotile content of the dust is variable and may indicate that chrysotile asbestos was not distributed uniformly during the three collapse events.

Bioreduction potentials of dried root of Zingiber officinale for a simple green synthesis of silver nanoparticles: Antibacterial studies.

PubMed

Judith Vijaya, J; Jayaprakash, N; Kombaiah, K; Kaviyarasu, K; John Kennedy, L; Jothi Ramalingam, R; Al-Lohedan, Hamad A; V M, Mansoor-Ali; Maaza, M

2017-12-01

Green synthesis of silver nanoparticles (Ag NPs) using an extract of dried Zingiber officinale (ginger) root as a reducing and capping agent in the presence of microwave irradiation was herein reported for the first time. The formation of symmetrical spheres is confirmed from the UV-Visible spectrum of Ag NPs. Fourier transform infra-red spectroscopy confirms the formation of the Ag NPs. X-ray diffraction analysis was utilized to calculate the crystallite size of Ag NPs and the value was found to be 10nm. High-resolution transmission electron microscopy and high-resolution scanning electron microscopy were used to investigate the morphology and size of the synthesized samples. The sphere like morphology is confirmed from the images. The purity and crystallinity of Ag NPs is confirmed by energy-dispersive X-Ray analysis and selected area electron diffraction respectively. The electrochemical behavior of the synthesized Ag NPs was assessed by cyclic voltammetry (CV) and shows the redox peaks in the potential range of -1.1 to +1.1V. Agar diffusion method is used to examine the antibacterial activity of Ag NPs. For this purpose, two gram positive and two gram negative bacteria were studied. This single step approach was found to be simple, short time, cost-effective, reproducible, and eco-friendly. Copyright © 2017. Published by Elsevier B.V.

Dijet production in $$\\sqrt{s}$$ = 7 TeV $pp$ collisions with large rapidity gaps at the ATLAS experiment

DOE PAGES

Aad, G.

2016-01-18

A 6.8 nb -1 sample of pp collision data collected under low-luminosity conditions at √s = 7 TeV by the ATLAS detector at the Large Hadron Collider is used to study diffractive dijet production. Events containing at least two jets with p T > 20 GeV are selected and analysed in terms of variables which discriminate between diffractive and non-diffractive processes. Cross sections are measured differentially in Δη F, the size of the observable forward region of pseudorapidity which is devoid of hadronic activity, and in an estimator, ξ¯, of the fractional momentum loss of the proton assuming single diffractivemore » dissociation (pp → pX). Model comparisons indicate a dominant non-diffractive contribution up to moderately large Δη F and small ξ¯, with a diffractive contribution which is significant at the highest Δη F and the lowest ξ¯. As a result, the rapidity-gap survival probability is estimated from comparisons of the data in this latter region with predictions based on diffractive parton distribution functions.« less

Structure and magnetic properties of SiO{sub 2}/PCL novel sol–gel organic–inorganic hybrid materials

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

Catauro, Michelina, E-mail: michelina.catauro@unina2.it; Bollino, Flavia; Cristina Mozzati, Maria

2013-07-15

Organic–inorganic nanocomposite materials have been synthesized via sol–gel. They consist of an inorganic SiO{sub 2} matrix, in which different percentages of poly(ε-caprolactone) (PCL) have been incorporated. The formation of H-bonds among the carbonyl groups of the polymer chains and Si–OH group of the inorganic matrix has been proved by means of Fourier transform infrared spectroscopy (FT-IR) analysis and has been confirmed by solid-state nuclear magnetic resonance (NMR). X-Ray diffraction (XRD) analysis highlighted the amorphous nature of the synthesized materials. Scanning electron microscope (SEM) micrograph and atomic force microscope (AFM) topography showed their homogeneous morphology and nanostructure nature. Considering the opportunitymore » to synthesize these hybrid materials under microgravity conditions by means of magnetic levitation, superconducting quantum interference device (SQUID) magnetometry has been used to quantify their magnetic susceptibility. This measure has shown that the SiO{sub 2}/PCL hybrid materials are diamagnetic and that their diamagnetic susceptibility is independent of temperature and increases with the PCL amount. - Graphical abstract: Characterization and magnetic properties of SiO{sub 2}/PCL organic–inorganic hybrid materials synthesized via sol–gel. FT-IR, Fourier transform infrared spectroscopy; solid-state NMR: solid-state nuclear magnetic resonance; SQUID: superconducting quantum interference device. - Highlights: • Sol–gel synthesis of SiO{sub 2}/PCL amorphous class I organic–inorganic hybrid materials. • FT-IR and NMR analyses show the hydrogen bonds formation between SiO{sub 2} and PCL. • AFM and SEM analyses confirm that the SiO{sub 2}/PCL are homogenous hybrid materials. • The SQUID measures show that the simples are diamagnetic. • Diamagnetic susceptibility of SiO{sub 2}/PCL materials increases with the PCL amount.« less

Silica Coating of Nonsilicate Nanoparticles for Resin-Based Composite Materials

PubMed Central

Kaizer, M.R.; Almeida, J.R.; Gonçalves, A.P.R.; Zhang, Y.; Cava, S.S.; Moraes, R.R.

2016-01-01

This study was designed to develop and characterize a silica-coating method for crystalline nonsilicate ceramic nanoparticles (Al2O3, TiO2, and ZrO2). The hypothesis was that the coated nonsilicate nanoparticles would stably reinforce a polymeric matrix due to effective silanation. Silica coating was applied via a sol-gel method, with tetraethyl orthosilicate as a silica precursor, followed by heat treatment. The chemical and microstructural characteristics of the nanopowders were evaluated before and after silica coating through x-ray diffraction, BET (Brunauer-Emmett-Teller), energy-dispersive x-ray spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy analyses. Coated and noncoated nanoparticles were silanated before preparation of hybrid composites, which contained glass microparticles in addition to the nanoparticles. The composites were mechanically tested in 4-point bending mode after aging (10,000 thermal cycles). Results of all chemical and microstructural analyses confirmed the successful obtaining of silica-coated nanoparticles. Two distinct aspects were observed depending on the type of nanoparticle tested: 1) formation of a silica shell on the surface of the particles and 2) nanoparticle clusters embedded into a silica matrix. The aged hybrid composites formulated with the coated nanoparticles showed improved flexural strength (10% to 30% higher) and work of fracture (35% to 40% higher) as compared with composites formulated with noncoated nanoparticles. The tested hypothesis was confirmed: silanated silica-coated nonsilicate nanoparticles yielded stable reinforcement of dimethacrylate polymeric matrix due to effective silanation. The silica-coating method presented here is a versatile and promising novel strategy for the use of crystalline nonsilicate ceramics as a reinforcing phase of polymeric composite biomaterials. PMID:27470069

Neutron powder diffraction studies as a function of temperature of structure II hydrate formed from propane

USGS Publications Warehouse

Rawn, C.J.; Rondinone, A.J.; Chakoumakos, B.C.; Circone, S.; Stern, L.A.; Kirby, S.H.; Ishii, Y.

2003-01-01

Neutron powder diffraction data confirm that hydrate samples synthesized with propane crystallize as structure type II hydrate. The structure has been modeled using rigid-body constraints to describe C3H8 molecules located in the eight larger polyhedral cavities of a deuterated host lattice. Data were collected at 12, 40, 100, 130, 160, 190, 220, and 250 K and used to calculate the thermal expansivity from the temperature dependence of the lattice parameters. The data collected allowed for full structural refinement of atomic coordinates and the atomic-displacement parameters.

Determination of the real structure of artificial and natural opals on the basis of three-dimensional reconstructions of reciprocal space

NASA Astrophysics Data System (ADS)

Eliseev, A. A.; Gorozhankin, D. F.; Napolskii, K. S.; Petukhov, A. V.; Sapoletova, N. A.; Vasilieva, A. V.; Grigoryeva, N. A.; Mistonov, A. A.; Byelov, D. V.; Bouwman, W. G.; Kvashnina, K. O.; Chernyshov, D. Yu.; Bosak, A. A.; Grigoriev, S. V.

2009-10-01

The distribution of the scattering intensity in the reciprocal space for natural and artificial opals has been reconstructed from a set of small-angle X-ray diffraction patterns. The resulting three-dimensional intensity maps are used to analyze the defect structure of opals. The structure of artificial opals can be satisfactorily described in the Wilson probability model with the prevalence of layers in the fcc environment. The diffraction patterns observed for a natural opal confirm the presence of sufficiently long unequally occupied fcc domains.

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.

Discrete diffraction managed solitons: Threshold phenomena and rapid decay for general nonlinearities

NASA Astrophysics Data System (ADS)

Choi, Mi-Ran; Hundertmark, Dirk; Lee, Young-Ran

2017-10-01

We prove a threshold phenomenon for the existence/non-existence of energy minimizing solitary solutions of the diffraction management equation for strictly positive and zero average diffraction. Our methods allow for a large class of nonlinearities; they are, for example, allowed to change sign, and the weakest possible condition, it only has to be locally integrable, on the local diffraction profile. The solutions are found as minimizers of a nonlinear and nonlocal variational problem which is translation invariant. There exists a critical threshold λcr such that minimizers for this variational problem exist if their power is bigger than λcr and no minimizers exist with power less than the critical threshold. We also give simple criteria for the finiteness and strict positivity of the critical threshold. Our proof of existence of minimizers is rather direct and avoids the use of Lions' concentration compactness argument. Furthermore, we give precise quantitative lower bounds on the exponential decay rate of the diffraction management solitons, which confirm the physical heuristic prediction for the asymptotic decay rate. Moreover, for ground state solutions, these bounds give a quantitative lower bound for the divergence of the exponential decay rate in the limit of vanishing average diffraction. For zero average diffraction, we prove quantitative bounds which show that the solitons decay much faster than exponentially. Our results considerably extend and strengthen the results of Hundertmark and Lee [J. Nonlinear Sci. 22, 1-38 (2012) and Commun. Math. Phys. 309(1), 1-21 (2012)].

Fluorescent light mediated a green synthesis of silver nanoparticles using the protein extract of weaver ant larvae.

PubMed

Khamhaengpol, Arunrat; Siri, Sineenat

2016-10-01

Alternative to crude plant extracts, a crude protein extract derived from animal cells is one of the potential sources of biomolecules for mediating a reduction of silver ions and a formation of silver nanoparticles (AgNPs) under a mild condition, which very few works have been reported. This work demonstrated a use of the protein extract of weaver ant larvae as a bio-facilitator for a simple, green synthesis of AgNPs under fluorescent light at room temperature. The protein extract of weaver ant larvae exhibited the reducing and antioxidant activities, which assisted a formation of AgNPs in the reaction containing only silver nitrate under light exposure. Transmission electron microscopy images revealed the dispersed, spherical AgNPs with an average size of 7.87±2.54nm. The maximum surface plasmon resonance (SPR) band of the synthesized AgNPs was at 435nm. The energy-dispersive X-ray analysis revealed that silver was a major element of the particles. The identity of AgNPs was confirmed by X-ray diffraction pattern, selected area electron diffraction and high resolution transmission electron microscopy analyses, which demonstrated the planes of face centered cubic silver. The synthesized AgNPs showed antibacterial activity against both Escherichia coli and Staphylococcus aureus with the minimum bactericidal concentration (MBC) values equally at 250μg/ml, suggesting their potential application as an effective antibacterial agent. Copyright © 2016 Elsevier B.V. All rights reserved.

Low energy electron diffraction and low energy electron microscopy microspot I/V analysis of the (4 x 4)O structure on Ag(111): surface oxide or reconstruction?

PubMed

Reichelt, R; Günther, S; Wintterlin, J; Moritz, W; Aballe, L; Mentes, T O

2007-10-07

A low energy electron diffraction (LEED) I/V analysis was performed of the (4 x 4) oxygen structure on Ag(111). Two data sets were used, one recorded with a conventional LEED system and a second with a low energy electron microscope (LEEM). The data sets agree well with each other, demonstrating that I/V structure analyses can be performed with the same quality with LEEM as with conventional LEED. The structure obtained confirms the recently proposed model that involves a reconstruction of the Ag(111) surface. Previous models based on a thin layer of Ag(2)O that had been accepted for more than 30 years are disproved. The reconstruction model contains two units of six triangularly arranged Ag atoms and a stacking fault in one half of the unit cell. The six O atoms per unit cell occupy sites in the trenches between the Ag(6) triangles. Small lateral displacements of the Ag atoms lift the mirror symmetry of the structure, leading to two nonequivalent groups of O atoms. The atoms of both groups are located approximately 0.5 Angstrom below the top Ag layer, on fourfold positions with respect to the top layer Ag atoms. Ag-O distances between 2.05 and 2.3 Angstrom are found. The oxygen atoms exhibit large static or dynamic displacements of up to 0.3 Angstrom at 300 K.

Quasi van der Waals epitaxy of copper thin film on single-crystal graphene monolayer buffer

NASA Astrophysics Data System (ADS)

Lu, Zonghuan; Sun, Xin; Washington, Morris A.; Lu, Toh-Ming

2018-03-01

Quasi van der Waals epitaxial growth of face-centered cubic Cu (~100 nm) thin films on single-crystal monolayer graphene is demonstrated using thermal evaporation at an elevated substrate temperature of 250 °C. The single-crystal graphene was transferred to amorphous (glass) and crystalline (quartz) SiO2 substrates for epitaxy study. Raman analysis showed that the thermal evaporation method had minimal damage to the graphene lattice during the Cu deposition. X-ray diffraction and electron backscatter diffraction analyses revealed that both Cu films are single-crystal with (1 1 1) out-of-plane orientation and in-plane Σ3 twin domains of 60° rotation. The crystallinity of the SiO2 substrates has a negligible effect on the Cu crystal orientation during the epitaxial growth, implying the strong screening effect of graphene. We also demonstrate the epitaxial growth of polycrystalline Cu on a commercial polycrystalline monolayer graphene consisting of two orientation domains offset 30° to each other. It confirms that the crystal orientation of the epitaxial Cu film follows that of graphene, i.e. the Cu film consists of two orientation domains offset 30° to each other when deposited on polycrystalline graphene. Finally, on the contrary to the report in the literature, we show that the direct current and radio frequency flip sputtering method causes significant damage to the graphene lattice during the Cu deposition process, and therefore neither is a suitable method for Cu epitaxial growth on graphene.

Crystal growth, differential gas adsorption, high thermal stability, and reversible coordination of two new barium-organic frameworks, Ba(SBA)(DMF){sub 4} and Ba{sub 2}(BTEC)(H{sub 2}O)

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

Halake, Shobha; Ok, Kang Min, E-mail: kmok@cau.ac.kr

2015-11-15

Single crystals of two barium-organic framework materials, Ba(SBA)(DMF){sub 4} (CAUMOF-15) and Ba{sub 2}(BTEC)(H{sub 2}O) (CAUMOF-16), have been grown through solvothermal reactions (H{sub 2}SBA=4,4′-sulfonyldibenzoic acid and H{sub 4}BTEC=1,2,4,5-benzenetetracarboxylic acid). The crystal structures of the reported frameworks have been determined by single-crystal X-ray diffraction. The materials have been fully characterized by powder X-ray diffraction (PXRD), elemental analyses, Infrared (IR) spectroscopy, and thermogravimetric analyses (TGA). CAUMOF-15 reveals a three-dimensional open-framework that comprises of an inorganic motif with one-dimensional chains and the SBA linkers. CAUMOF-16 shows another three-dimensional backbone consisting of layers of edge-shared BaO{sub 9} and BaO{sub 10} polyhedra, and BTEC pillars. Bothmore » of the 3D frameworks exhibit relatively high thermal stabilities. The PXRD and IR spectral data confirm that CAUMOF-15 and CAUMOF-16 reveal reversible coordinations of the respective solvent molecules, DMF and H{sub 2}O. Gas adsorption properties towards nitrogen, hydrogen, and carbon dioxide have been also investigated. - Graphical abstract: Crystals of two new barium-organic frameworks, Ba(SBA)(DMF){sub 4} and Ba{sub 2}(BTEC)(H{sub 2}O), exhibiting a differential gas adsorption, a high thermal stability, and a reversible coordination of solvent molecules have been grown. - Highlights: • Crystals of two new 3D Ba-MOFs are grown. • The two Ba-MOFs reveal very high thermal stabilities up to ca. 400 °C. • Ba(SBA)(DMF){sub 4} exhibits differential gas adsorption properties. • The two Ba-MOFs show reversible coordination of the solvent molecules.« less

Synthesis, characterization, and antifungal activity of novel (Z)-N-(2-cyano-3-phenylprop-2-en-1-yl)-alkyl/aryl-sulfonamides derived from a Morita-Baylis-Hillman adduct

NASA Astrophysics Data System (ADS)

Tavares, Eder C.; Rubinger, Mayura M. M.; Zacchi, Carlos H. C.; Silva, Simone A.; Oliveira, Marcelo R. L.; Guilardi, Silvana; Alcântara, Antônio F. de C.; Piló-Veloso, Dorila; Zambolim, Laércio

2014-06-01

A series of allyl sulfonamides prepared from the reaction of the Morita-Baylis-Hillman adduct 2-[hydroxy(phenyl)methyl]acrylonitrile with primary sulfonamides (RSO2NH2), where R = C6H5 (1), 4-Fsbnd C6H4 (2), 4-Clsbnd C6H4 (3), 4-Brsbnd C6H4 (4), 4-NO2sbnd C6H4 (5), CH3 (6), CH3CH2 (7), CH3(CH2)3 (8), and CH3(CH2)7 (9), were characterized by IR, 1H and 13C NMR spectroscopies, mass spectrometry and elemental analyses. BLYP/6-31G* calculations suggested stereoselective reactions, resulting in the exclusive formation of the thermodynamically more stable Z-products. The Z-configuration of the products was confirmed by NOE difference spectroscopy and single crystal X-ray diffraction measurements. The allyl sulfonamides were active against Colletotrichum gloeosporioides, an important agent of anthracnose in plants.

3D Interconnected Binder-Free Electrospun MnO@C Nanofibers for Supercapacitor Devices.

PubMed

Ramadan, Mohamed; Abdellah, Ahmed M; Mohamed, Saad G; Allam, Nageh K

2018-05-22

Rational design of binder-free materials with high cyclic stability and high conductivity is a great need for high performance supercapacitors. We demonstrate a facile one-step synthesis method of binder-free MnO@C nanofibers as electrodes for supercapacitor applications. The topology of the fabricated nanofibers was investigated using FESEM and HRTEM. The X-ray photoelectron spectroscopy (XPS) and the X-ray diffraction (XRD) analyses confirm the formation of the MnO structure. The electrospun MnO@C electrodes achieve high specific capacitance of 578 F/g at 1 A/g with an outstanding cycling performance. The electrodes also show 127% capacity increasing after 3000 cycles. An asymmetric supercapacitor composed of activated carbon as the negative electrode and MnO@C as the positive electrode shows an ultrahigh energy density of 35.5 Wh/kg with a power density of 1000 W/kg. The device shows a superior columbic efficiency, cycle life, and capacity retention.

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

PubMed

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

2014-05-05

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

Brown algae hydrolysis in 1-n-butyl-3-methylimidazolium chloride with mineral acid catalyst system.

PubMed

Malihan, Lenny B; Nisola, Grace M; Chung, Wook-Jin

2012-08-01

The amenability of three brown algal species, Sargassum fulvellum, Laminaria japonica and Undaria pinnatifida, to hydrolysis were investigated using the ionic liquid (IL), 1-n-butyl-3-methylimidazolium chloride ([BMIM]Cl). Compositional analyses of the brown algae reveal that sufficient amounts of sugars (15.5-29.4 wt.%) can be recovered. Results from hydrolysis experiments show that careful selection of the type of mineral acid as catalyst and control of acid loading could maximize the recovery of sugars. Optimal reaction time and temperature were determined from the kinetic studies on the sequential reducing sugar (TRS) formation and degradation. Optimal reaction times were determined based on the extent of furfurals formation as TRS degradation products. X-ray diffraction and environmental scanning electron microscopy confirmed the suitability of [BMIM]Cl as solvent for the hydrolysis of the three brown algae. Overall results show the potential of brown algae as renewable energy resources for the production of valuable chemicals and biofuels. Copyright © 2012 Elsevier Ltd. All rights reserved.

Biogenic copper oxide nanoparticles synthesis using Tabernaemontana divaricate leaf extract and its antibacterial activity against urinary tract pathogen

NASA Astrophysics Data System (ADS)

Sivaraj, Rajeshwari; Rahman, Pattanathu K. S. M.; Rajiv, P.; Salam, Hasna Abdul; Venckatesh, R.

2014-12-01

This investigation explains the biosynthesis and characterization of copper oxide nanoparticles from an Indian medicinal plant by an eco-friendly method. The main objective of this study is to synthesize copper oxide nanoparticles from Tabernaemontana divaricate leaves through a green chemistry approach. Highly stable, spherical copper oxide nanoparticles were synthesized by using 50% concentration of Tabernaemontana leaf extract. Formation of copper oxide nanoparticles have been characterized by UV-Vis absorption spectroscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDX) and transmission electron microscopy (TEM) analysis. All the analyses revealed that copper oxide nanoparticles were 48 ± 4 nm in size. Functional groups and chemical composition of copper oxide were also confirmed. Antimicrobial activity of biogenic copper oxide nanoparticles were investigated and maximum zone of inhibition was found in 50 μg/ml copper oxide nanoparticles against urinary tract pathogen (Escherichia coli).

A biosensor system using nickel ferrite nanoparticles

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

Singh, Prachi, E-mail: prachi.singh@st.niituniversity.in; Rathore, Deepshikha, E-mail: deep.nano@gmail.com

2016-05-06

NiFe{sub 2}O{sub 4} ferrite nanoparticles were synthesized by chemical co-precipitation method and the structural characteristics were investigated using X-ray diffraction technique, where single cubic phase formation of nanoparticles was confirmed. The average particle size of NiFe{sub 2}O{sub 4} was found to be 4.9 nm. Nanoscale magnetic materials are an important source of labels for biosensing due to their strong magnetic properties which are not found in biological systems. This property of the material was exploited and the fabrication of the NiFe{sub 2}O{sub 4} nanoparticle based biosensor was done in the form of a capacitor system, with NiFe{sub 2}O{sub 4} as themore » dielectric material. The biosensor system was tested towards different biological materials with the help of electrochemical workstation and the same was analysed through Cole-Cole plot of NiFe{sub 2}O{sub 4}. The performance of the sensor was determined based on its sensitivity, response time and recovery time.« less

Tuning effect of polysaccharide Chitosan on structural, morphological, optical and photoluminescence properties of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Magesh, G.; Bhoopathi, G.; Nithya, N.; Arun, A. P.; Ranjith Kumar, E.

2018-05-01

Chitosan/ZnO nanocomposites was synthesized by in-situ chemical precipitation method. The effect of polysaccharide Chitosan concentration (0.1 g, 0.5 g, 1 g and 3 g) was investigated by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) with Energy dispersive spectroscopy (EDX), High Resolution Transmission Electron Microscopy (HRTEM), UV-visible (UV), Fourier Transform Infrared (FTIR) and Photoluminescence Spectroscopy (PL). XRD pattern confirms the hexagonal wurtzite structure of the Chitosan/ZnO nanocomposites. The structural morphology and the elemental composition of the samples were analysed by FESEM and EDX respectively. From TEM analysis, it is observed that the particles in spindle shape morphology with average particle size ranges 10-20 nm. UV-Vis analysis reveals that the Chitosan concentration affect the absorption band edge and shift towards lower wavelength. The oxygen vacancy induced photoluminescence of ZnO nanoparticles was observed and its intensity decreases by tuning the Chitosan concentration.

Microwave-assisted Bi2Se3 nanoparticles using various organic solvents

NASA Astrophysics Data System (ADS)

Vijila, J. Joy Jeba; Mohanraj, K.; Henry, J.; Sivakumar, G.

2016-01-01

Microwave assisted Bi2Se3 nanoparticles were synthesized from five different solvents DMF, EG, EG + H2O, EDA + dil.HNO3 and N2H4 + H2O + Ethanol. The influence of solvents on purity of the compound was analysed by using X-ray diffraction patterns. The result indicates pure rhombohedral Bi2Se3 nanoparticles formed for N2H4 + H2O + Ethanol. The presence of vibrational bands in the range of 400-800 cm- 1 is confirmed the formation of Bi2Se3. The maximum optical absorption observed around 450 nm and the band gap values are found in the range of 1.5 eV-2.17 eV for all the solvents. The nanostructure of the Bi2Se3 particles change with solvents. From the experimental results, the solvent N2H4 + H2O + Ethanol produces pure nanosize Bi2Se3 particles under the microwave assisted method.

Synthesis, structural and vibrational studies on mixed alkali metal gadolinium double tungstate, K1-xNaxGd(WO4)2

NASA Astrophysics Data System (ADS)

Durairajan, A.; Thangaraju, D.; Moorthy Babu, S.

2013-02-01

Mixed alkali double tungstates K1-xNaxGd(WO4)2 (KNGW) (0 ⩽ x ⩽ 1) were synthesized by solid state reaction using sodium doped monoclinic KGd(WO4)2 (KGW). Synthesized KNGW powders were characterized using powder X-ray diffraction (XRD), differential thermal analysis (DTA), scanning electron microscopy (SEM) and Raman analysis. DTA analysis confirms that the melting point of the KGW matrix increases from 1063 °C to 1255 °C with increasing sodium content. The Powder XRD analyses reveal that mixed phases were observed up to 40 wt.% of Na in the KGW matrix above that percentage there is domination of scheelite structure in the synthesized powder. Polyhedral type, bi-pyramidal shape and spheroid shape morphology was observed for KGW, NKGW and NGW powders respectively. The Raman analysis was carried out to understand the vibrational characteristic changes with mixing of sodium ions in the KGW matrix.

A comparative study on the crystal structure of bicycle analogues to the natural phytotoxin helminthosporins

NASA Astrophysics Data System (ADS)

Barbosa, Luiz Cláudio de Almeida; Teixeira, Robson Ricardo; Nogueira, Leonardo Brandão; Maltha, Celia Regina Alvares; Doriguetto, Antônio Carlos; Martins, Felipe Terra

2016-02-01

Herein we described structural insights of a series of analogues to helminthosporin phytotoxins. The key reaction used to prepare the compounds corresponded to the [3 + 4] cycloaddition between the oxyallyl cation generated from 2,4-dibromopentan-3-one and different furans. Their structures were confirmed upon IR, NMR and X-ray diffraction analyses. While bicycles 7, 8 and 9 crystallize in the centrosymmetric monoclinic space group P21/c, compound 10 was solved in the noncentrosymmetric orthorhombic space group P212121. The solid materials obtained were shown to be racemic crystals (7, 8, 9) or racemic conglomerate (10). In all compounds, there is formation of a bicycle featured by fused tetrahydropyranone and 2,5-dihydrofuran rings. They adopt chair and envelope conformations, respectively. Crystal packing of all compounds is stabilized through C-H•••O contacts. Conformational aspects as well as similarities and differences among the crystal structures of the synthesized analogues are discussed.

Electrical properties of fullerenol C{sub 60}(OH){sub 10}/Au interface

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

Sakaino, Masamichi, E-mail: sun@ele.kyutech.ac.jp; Sun, Yong; Morimoto, Fumio

Electrical properties of the C{sub 60}(OH){sub 10}/Au contact have been studied by measuring its current-voltage characteristics in the temperature range of 300–500 K. The Schottky barrier of the C{sub 60}(OH){sub 10}/Au contact was confirmed to be 0.70±0.02 eV from Arrhenius plots of the current-voltage characteristics measured at various bias voltages as well as various preparation conditions of the C{sub 60}(OH){sub 10} material. Significant effect of the applied electric field on the barrier height has not been observed in the range of 0.1–2.0 MVm{sup −1}. The effects of both the charge transfer from C{sub 60} cage to OH groups and the crystallinity of themore » C{sub 60}(OH){sub 10} material on the Schottky barrier were discussed on the basis of x-ray photoemission spectroscopy and x-ray diffraction analyses.« less

Phosphorus K-edge XANES spectroscopy of mineral standards

PubMed Central

Ingall, Ellery D.; Brandes, Jay A.; Diaz, Julia M.; de Jonge, Martin D.; Paterson, David; McNulty, Ian; Elliott, W. Crawford; Northrup, Paul

2011-01-01

Phosphorus K-edge X-ray absorption near-edge structure (XANES) spectroscopy was performed on phosphate mineral specimens including (a) twelve specimens from the apatite group covering a range of compositional variation and crystallinity; (b) six non-apatite calcium-rich phosphate minerals; (c) 15 aluminium-rich phosphate minerals; (d) ten phosphate minerals rich in either reduced iron or manganese; (e) four phosphate minerals rich in either oxidized iron or manganese; (f) eight phosphate minerals rich in either magnesium, copper, lead, zinc or rare-earth elements; and (g) four uranium phosphate minerals. The identity of all minerals examined in this study was independently confirmed using X-ray powder diffraction. Minerals were distinguished using XANES spectra with a combination of pre-edge features, edge position, peak shapes and post-edge features. Shared spectral features were observed in minerals with compositions dominated by the same specific cation. Analyses of apatite-group minerals indicate that XANES spectral patterns are not strongly affected by variations in composition and crystallinity typical of natural mineral specimens. PMID:21335905

Facile synthesis of lithium sulfide nanocrystals for use in advanced rechargeable batteries

DOE PAGES

Li, Xuemin; Wolden, Colin A.; Ban, Chunmei; ...

2015-12-03

This work reports a new method of synthesizing anhydrous lithium sulfide (L i2S) nanocrystals and demonstrates their potential as cathode materials for advanced rechargeable batteries. Li 2S is synthesized by reacting hydrogen sulfide (H 2S) with lithium naphthalenide (Li-NAP), a thermodynamically spontaneous reaction that proceeds to completion rapidly at ambient temperature and pressure. The process completely removes H 2S, a major industrial waste, while cogenerating 1,4-dihydronaphthalene, itself a value-added chemical that can be used as liquid fuel. The phase purity, morphology, and homogeneity of the resulting nanopowders were confirmed by X-ray diffraction and scanning electron microscopy. The synthesized Li 2Smore » nanoparticles (100 nm) were assembled into cathodes, and their performance was compared to that of cathodes fabricated using commercial Li 2S micropowders (1–5 μm). As a result, electrochemical analyses demonstrated that the synthesized Li 2S were superior in terms of (dis)charge capacity, cycling stability, output voltage, and voltage efficiency.« less

The effect of bismuth on the structure, magnetic and electric properties of Co2MnO4 spinel multiferroic

NASA Astrophysics Data System (ADS)

Chouaya, H.; Smari, M.; Walha, I.; Dhahri, E.; Graça, M. P. F.; Valente, M. A.

2018-04-01

Mixed Co2Mn1-xBixO4 (x = 0, x = 0.05 and x = 0.1) samples were prepared by the sol-gel method using the citric acid route and characterized by various techniques. The X-ray diffraction (XRD) and Raman spectroscopic analyses confirmed the formation of inverse spinel cubic structure with Fd 3 ‾ m space group. The introduction of Bismuth (Bi) into Co2MnO4 did not modify the ferrimagnetic character of the parent compound Co2MnO4, whereas the field-cooled magnetizations MFC and the Curie temperature Tc decreased when increasing the Bi content. The electrical properties showed an activation energy (Ea) increase caused by the decrease of the double-exchange interaction following the substitution of Mn3+ by Bi3+. Eventually, the temperature coefficient of resistance (TCR) shows significant values for all samples can be investigated also as good candidates for bolometer applications.

Characterisation of bare and tannase-loaded calcium alginate beads by microscopic, thermogravimetric, FTIR and XRD analyses.

PubMed

Larosa, Claudio; Salerno, Marco; de Lima, Juliana Silva; Merijs Meri, Remo; da Silva, Milena Fernandes; de Carvalho, Luiz Bezerra; Converti, Attilio

2018-08-01

Incorporating enzymes into calcium alginate beads is an effective method to immobilise them and to preserve, at the same time, their catalytic activity. Sodium alginate was mixed with Aspergillus ficuum tannase in aqueous solution, and tannase-loaded calcium alginate beads were prepared using a simple droplet-based microfluidic system. Extensive experimental analysis was carried out to characterise the samples. Microscopic imaging revealed morphological differences between the surfaces of bare alginate matrix and tannase-loaded alginate beads. Thermal analysis allowed assessing the hydration contents of alginate and revealed the presence of tannase entrapped in the loaded beads, which was confirmed by vibrational spectroscopy. X-ray diffraction allowed us to conclude that alginate of tannase-loaded beads is not crystalline, which would make them suitable as carriers for possible controlled release. Moreover, they could be used in food applications to improve tea quality or clarify juices. Copyright © 2018 Elsevier B.V. All rights reserved.

Novel synthesis of cobalt/poly vinyl alcohol/gamma alumina nanocomposite for catalytic application

NASA Astrophysics Data System (ADS)

Hatamie, Shadie; Ahadian, Mohammad Mahdi; Rashidi, Alimoradeh; Karimi, Ali; Akhavan, Omid

2017-05-01

In this manuscript, synthesis of cobalt/poly vinyl alcohol (PVA)/gamma alumina nanocomposite via a simple room temperature, as well as its catalyst performance were explored. Brunauer-Emmett-Teller analysis, X-ray diffraction, X-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy were conducted. The surface area of the polymeric composite was obtained to be 280 m2/g. The cobalt loading on the nanocomposite was measured using inductivity couple plasma. Transmission electron microscopy analysis showed that the size of cobalt crystalline encapsulate inside the polymer was confined to 5 nm. Magnetic property analysis, using vibrating sample magnetometer, confirmed ferromagnetic nature of the composite. Thermo-gravimetric analyses were employed to explain the degradation process for the polymeric base nanocomposite. Temperature-programmed reduction was used to evaluate the structural form of cobalt oxide in nanocomposite. The catalysis activity was determined by Fischer-Tropsch synthesize, which showed a high catalyst selectivity to C2-C4 hydrocarbons.

New Ni-based quaternary disk-shaped catalysts for low-temperature CO2 methanation: Fabrication, characterization, and performance.

PubMed

Moon, Dea Hyun; Lee, Sang Moon; Ahn, Jeong Yoon; Nguyen, Dinh Duc; Kim, Sung Su; Chang, Soon Woong

2018-07-15

Ni-based quaternary disk catalysts were manufactured for low-temperature CO 2 methanation reactions, and the reaction activity was examined with respect to the thermal treatment conditions. By applying varying reduction and combustion treatments, the same catalysts were compared, and the Ni oxidation conditions and physical features were confirmed through X-Ray diffraction, scanning electron microscopy, and energy dispersive X-ray analyses. In addition, oxygen adsorption/desorption changes were measured by temperature-programmed reduction after pre-treating with oxygen and hydrogen. The reduction treatment catalyst showed a conversion of 20% at 280 °C, and the 70% calcined catalyst did not form a NiO crystalloid. The activation of the catalyst increased because of NiO movement on the catalyst surface, which enabled easy transformation to metallic Ni. The prepared catalyst is a highly reactive, yet stable, candidate for practical catalytic CO 2 methanation. Copyright © 2018 Elsevier Ltd. All rights reserved.

Exfoliation of non-oxidized graphene flakes for scalable conductive film.

PubMed

Park, Kwang Hyun; Kim, Bo Hyun; Song, Sung Ho; Kwon, Jiyoung; Kong, Byung Seon; Kang, Kisuk; Jeon, Seokwoo

2012-06-13

The increasing demand for graphene has required a new route for its mass production without causing extreme damages. Here we demonstrate a simple and cost-effective intercalation based exfoliation method for preparing high quality graphene flakes, which form a stable dispersion in organic solvents without any functionalization and surfactant. Successful intercalation of alkali metal between graphite interlayers through liquid-state diffusion from ternary KCl-NaCl-ZnCl(2) eutectic system is confirmed by X-ray diffraction and X-ray photoelectric spectroscopy. Chemical composition and morphology analyses prove that the graphene flakes preserve their intrinsic properties without any degradation. The graphene flakes remain dispersed in a mixture of pyridine and salts for more than 6 months. We apply these results to produce transparent conducting (∼930 Ω/□ at ∼75% transmission) graphene films using the modified Langmuir-Blodgett method. The overall results suggest that our method can be a scalable (>1 g/batch) and economical route for the synthesis of nonoxidized graphene flakes.

Synthesis, structure and characterization of a hybrid centrosymmetric material (4-dimethylaminopyridinium nitrate gallic acid monohydrate) well-designed for non-linear optics

NASA Astrophysics Data System (ADS)

Ennaceur, Nasreddine; Jalel, Boutheina; Henchiri, Rokaya; Cordier, Marie; Ledoux-Rak, Isabelle

2018-01-01

Hybrid material: 4-Dimethylaminopyridinium nitrate gallic acid monohydrate abbreviated DNGA monohydrate has been successfully synthesized by slow evaporation method at room temperature. X-ray diffraction (XRD) on a single crystal showed that the latter was crystallized in P-1 space group. Likewise, thermal analyses demonstrated the stability of our crystal up to 80 °C. Besides, the analysis of the infrared spectrum (FTIR), allowed us to confirm the presence of the different groups present in the structure. Furthermore, by studying the UV-Visible spectrum, the transparency of our crystal was proven. Despite the fact that of having a centrosymmetric structure, the nonlinear optical properties of our single crystal, which was tested by Kurtz-Perry technique, proved that its second harmonic generation efficiency was 1.22 times more than that of KDP (potassium dihydrogen phosphate) single crystal. This nonlinear optical behavior of the studied compound was also determined through the calculations of polarizability and first hyperpolarizability values.

Template-Free Synthesis and Enhanced Photocatalytic Performance of Uniform BiOCI Flower-Like Microspheres.

PubMed

Chang, Fei; Xie, Yunchao; Chen, Juan; Luo, Jieru; Li, Chenlu; Hu, Xuefeng; Xu, Bin

2015-02-01

Preparation of uniform BiOCI flower-like microspheres was facilely accomplished through a sim- ple protocol involving regulation of pH value in aqueous with sodium hydroxide in the presence of n-propanol. The as-prepared samples were characterized by a collection of techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), UV-vis diffuse reflectance spectroscopy (UV-vis DRS), and nitrogen adsorption-desorption isotherms. Based upon the SEM analyses, uniform microspheres could be formed with coexistence of some fragments of BiOCI nanosheets without n-propanol. The addition of appropriate amount of n-propanol was beneficial to provide BiOCI samples containing only flower-like microspheres, which were further subjected to the photocatalytic measurements towards Rhodamine B in aqueous under visible light irradiation and exhibited the best catalytic performance among all samples tested. In addition, the photocatalytic process was confirmed to undergo through a photosensitization pathway, in which superoxide radicals (.O-) played critical roles.

Structure, Elastic Constants and XRD Spectra of Extended Solids under High Pressure

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

Batyrev, I. G.; Coleman, S. P.; Ciezak-Jenkins, J. A.

We present results of evolutionary simulations based on density functional calculations of a potentially new type of energetic materials called extended solids: P-N and N-H. High-density structures with covalent bonds generated using variable and fixed concentration methods were analysed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction (XRD) spectra. X-ray diffraction spectra were calculated using a virtual diffraction algorithm that computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculated XRD patterns were used to search for the structure of extended solids present at experimental pressures by optimizing data accordingmore » to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Elastic constants has been calculated for thermodynamically stable structures of P-N system.« less

Thermal expansion in UO 2 determined by high-energy X-ray diffraction

DOE PAGES

Guthrie, M.; Benmore, C. J.; Skinner, L. B.; ...

2016-06-24

In this study, we present crystallographic analyses of high-energy X-ray diffraction data on polycrystalline UO 2 up to the melting temperature. The Rietveld refinements of our X-ray data are in agreement with previous measurements, but are systematically located around the upper bound of their uncertainty, indicating a slightly steeper trend of thermal expansion compared to established values. This observation is consistent with recent first principles calculations.

Occurrence and characterisation of calcium oxalate crystals in stems and fruits of Hylocereus costaricensis and Selenicereus megalanthus (Cactaceae: Hylocereeae).

PubMed

Viñas, María; Jiménez, Víctor M

2016-10-01

Detailed description about occurrence of calcium oxalate (CaOx) crystals in the edible vine cactus species Hylocereus costaricensis and Selenicereus megalanthus is scarce. Therefore, we evaluated and characterized the presence, morphology and composition of CaOx crystals in both species. Crystals were isolated from greenhouse and in vitro vegetative stems, and from ripe fruit peels and pulp by enzymatic digestion and density centrifugation and quantified with a haemocytometer. Morphologies were studied using scanning electron microscopy, elemental composition with energy-dispersive X-ray spectroscopy and salt composition with X-ray powder diffraction. Analyses conducted confirmed that isolated crystals were exclusively composed by CaOx, both mono- and dihydrated. Highest crystal contents were measured in greenhouse stems, followed by the fruit peels. While very few crystals were quantified in in vitro plants, they were not detected in the fruit pulp at all, which is of advantage for its human consumption and could be linked to mechanisms of seed dispersal through animals. Different crystal morphologies were observed, sometimes varying between genotypes and tissues analysed. This is the first work known to the authors with a detailed characterization of CaOx crystals in vine cacti. Copyright © 2016 Elsevier Ltd. All rights reserved.

Polyethylene Films Containing Silver Nanoparticles for Applications in Food Packaging: Characterization of Physico-Chemical and Anti-Microbial Properties.

PubMed

Becaro, Aline A; Puti, Fernanda C; Correa, Daniel S; Paris, Elaine C; Marconcini, José M; Ferreira, Marcos D

2015-03-01

This paper reports the antibacterial effect and physico-chemical characterization of films containing silver nanoparticles for use as food packaging. Two masterbatches (named PEN and PEC) con- taining silver nanoparticles embedded in distinct carriers (silica and titanium dioxide) were mixed with low-density polyethylene (LDPE) in different compositions and extruded to produce plain films. These films were characterized by Scanning Electron Microscopy (SEM), X-ray diffraction (XRD), Differential Scanning Calorimetry (DSC), Thermogravimetric analysis (TGA) and Fourier Transform Infrared Spectroscopy (FTIR). The morphology of the films showed the formation of agglomerates of nanoparticles in both PEN and PEC composites. X-ray analyses confirmed the presence of SiO2 in PEN samples and TiO2 in PEC samples. Thermal analyses indicated an increase in thermal stability of the PEC compositions. The antimicrobial efficacy was determined by applying the test strain for Escherichia coli and Staphylococcus aureus, according to the Japanese Industrial Standard Method (JIS Z 2801:2000). The films analyzed showed antimicrobial properties against the tested microorganisms, presenting better activity against the S. aureus than E. Coli. These findings suggest that LDPE films with silver nanoparticles are promising to provide a significant contribution to the quality and safety of packaged food.

Electrical, dielectric properties and study of AC electrical conduction mechanism of Li0.9□0.1NiV0.5P0.5O4

NASA Astrophysics Data System (ADS)

Rahal, A.; Borchani, S. Megdiche; Guidara, K.; Megdiche, M.

2018-02-01

In this paper, we report the measurements of impedance spectroscopy for a new olivine-type lithium deficiency Li0.9□0.1NiV0.5P0.5O4 compound. It was synthesized by the conventional solid-state technique. All the X-ray diffraction peaks of the compound are indexed, and it is found that the sample is well crystallized in orthorhombic olivine structure belonging to the space group Pnma. Conductivity and dielectric analyses of the sample are carried out at different temperatures and frequencies using the complex impedance spectroscopy technique. The electrical conductivity of Li0.9□0.1NiV0.5P0.5O4 is higher than that of parent compound LiNiV0.5P0.5O4. Temperature dependence of the DC conductivity and modulus was found to obey the Arrhenius law. The obtained values of activation energy are different which confirms that transport in the title compound is not due to a simple hopping mechanism. To determine the conduction mechanism, the AC conductivity and its frequency exponent have been analysed in this work by a theoretical model based on quantum mechanical tunnelling: the non-overlapping small polaron tunnelling model.

A facile pollutant-free approach toward a series of nutritionally effective calcium phosphate nanomaterials for food and drink additives

NASA Astrophysics Data System (ADS)

Wang, Jieru; Chen, Xiaoyi; Yang, Xianyan; Xu, Sanzhong; Zhang, Xinli; Gou, Zhongru

2011-03-01

Micronutrient malnutrition is widespread and constitutes one of the main nutritional problems worldwide. Vitamins, amino acids, carbohydrates and Ca-phosphate (CaP) minerals are important to human health and disease prevention. Herein we developed a simple wet-chemical method to prepare multinary nutrients-containing CaP nanomaterials in diluted apple, orange, and grape juices. The scanning electron microscopy observation shows that these nanomaterials are short plate-like CaP nanocrystals of 500 nm in length. The X-ray photoelectron spectroscopy, nitrogen adsorption, thermogravimetric analyses confirm the different specific surface area and organic nutrient contents. The Fourier transform infrared and X-ray diffraction analyses indicate there exist similar organic groups (i.e., COO-, HN-CO) but different CaP species in the precipitates. The dissolution test in vitro simulated stomach juice pH condition indicates that these inorganic-organic nanohybrid materials are multidoped by micronutrients (such as Zn, Sr, Mg, K, vitamin c) and can be readily dissolved in the weak acidic aqueous solutions. This highly efficient utilization of fruit juice to produce CaP-based micronutrient composites may minimize the adverse side effect, so that the nanomaterials are promising as functional food/drink additives. Thus, this novel approach is environmentally and biologically friendly to produce edible nutrients while production cost is attained.

Method for determining the composition and orientation of III-V {001} semiconductor surfaces

NASA Astrophysics Data System (ADS)

Sung, M. M.; Kim, C.; Rabalais, J. W.

1996-09-01

A method for determining the composition and orientation of III-V {001} semiconductor surfaces is presented and applications are described. The information is obtained from the techniques of time-of-flight scattering and recoiling spectrometry (TOF-SARS), using the composition from azimuth-specific elemental accessibilities (CASEA) method, and low energy electron diffraction (LEED). The azimuth-specific elemental accessibilities (ASEA) are measured experimentally and calculated from the number of accessible atoms in the unit cell and from three-dimensional trajectory simulations using the SARIC program. The in situ analyses identify the 1st-layer elemental species and determine the orientation of the reconstructed surface symmetry elements with respect to the bulk crystallographic directions. This is demonstrated for the III-V {001} compound semiconductor surfaces of GaAs and InAs in the (4 × 2) and (4 × 2) phases and InP in the (4 × 2) phase. The analyses confirm the missing-row-dimer (MRD) structure for GaAs and InAs in which the missing row direction is parallel to the direction of the 1st-layer multimers (dimers) and the missing-row-trimer-dimer (MRTD) structure for InP in which the missing row direction is perpendicular to the direction of the 1st-layer multimers (trimers).

Growth and characterization of barium complex of 1,3,5-triazinane-2,4,6-trione in gel: a corrosion inhibiting material

NASA Astrophysics Data System (ADS)

Divya, R.; Nair, Lekshmi P.; Bijini, B. R.; Nair, C. M. K.; Babu, K. Rajendra

2018-05-01

Good quality prismatic crystals of industrially applicable corrosion inhibiting barium complex of 1,3,5-triazinane-2,4,6-trione have been grown by conventional gel method. The crystal structure, packing, and nature of bonds are revealed in the single crystal X-ray diffraction analysis. The crystal has a three-dimensional polymeric structure having a triclinic crystal system with the space group P-1. The powder X-ray diffraction analysis confirms its crystalline nature. The functional groups present in the crystal are identified by Fourier transform infrared spectroscopy. Elemental analysis confirms the stoichiometry of the elements present in the complex. Thermogravimetric analysis and differential thermal analysis reveal its good thermal stability. The optical properties like band gap, refractive index and extinction coefficient are evaluated from the UV-visible spectral analysis. The singular property of the material, corrosion inhibition efficiency achieved by the adsorption of the sample molecules is determined by the weight loss method.

Facile fabrication of BiVO4 nanofilms with controlled pore size and their photoelectrochemical performances

NASA Astrophysics Data System (ADS)

Feng, Chenchen; Jiao, Zhengbo; Li, Shaopeng; Zhang, Yan; Bi, Yingpu

2015-12-01

We demonstrate a facile method for the rational fabrication of pore-size controlled nanoporous BiVO4 photoanodes, and confirmed that the optimum pore-size distributions could effectively absorb visible light through light diffraction and confinement functions. Furthermore, in situ X-ray photoelectron spectroscopy (XPS) reveals more efficient photoexcited electron-hole separation than conventional particle films, induced by light confinement and rapid charge transfer in the inter-crossed worm-like structures.We demonstrate a facile method for the rational fabrication of pore-size controlled nanoporous BiVO4 photoanodes, and confirmed that the optimum pore-size distributions could effectively absorb visible light through light diffraction and confinement functions. Furthermore, in situ X-ray photoelectron spectroscopy (XPS) reveals more efficient photoexcited electron-hole separation than conventional particle films, induced by light confinement and rapid charge transfer in the inter-crossed worm-like structures. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr06584d

Step-by-step fabrication of a highly oriented crystalline three-dimensional pillared-layer-type metal-organic framework thin film confirmed by synchrotron X-ray diffraction.

PubMed

Otsubo, Kazuya; Haraguchi, Tomoyuki; Sakata, Osami; Fujiwara, Akihiko; Kitagawa, Hiroshi

2012-06-13

Fabrication of a crystalline ordered thin film based on the porous metal-organic frameworks (MOFs) is one of the practical applications of the future functional nanomaterials. Here, we report the creation of a highly oriented three-dimensional (3-D) porous pillared-layer-type MOF thin film on a metal substrate using a step-by-step approach based on liquid-phase epitaxy. Synchrotron X-ray diffraction (XRD) study clearly indicates that the thin film is crystalline and its orientation is highly controlled in both horizontal and vertical directions relative to the substrate. This report provides the first confirmation of details of not only the crystallinity but also the orientation of 3-D MOF thin film using synchrotron XRD. Moreover, we also demonstrate its guest adsorption/desorption behavior by using in situ XRD measurements. The results presented here would promise useful insights for fabrication of MOF-based nanodevices in the future.

Study of magnetic behavior in hexagonal-YMn1-xFexO3 (x=0 and 0.2) nanoparticles using remanent magnetization curves

NASA Astrophysics Data System (ADS)

Chauhan, Samta; Singh, Amit Kumar; Srivastava, Saurabh Kumar; Chandra, Ramesh

2016-09-01

We have studied the magnetic behavior of YMn1-xFexO3 (x=0 and 0.2) nanoparticles synthesized by conventional solid state reaction method. The as-synthesized nanoparticles were found to have hexagonal phase with P63cm space group confirmed by X-Ray diffraction. The particle size was found to be ~70 nm as confirmed by both X-Ray diffraction and Transmission Electron Microscopy. DC magnetization and memory effect measurements imply that the h-YMnO3 nanoparticles bear a resemblance to super spin-glass state following de Almeida-Thouless like behavior which is being suppressed by Fe-doping. The Fe-doping in YMnO3 enhances the antiferromagnetic (AFM) transition temperature TN to ~79 K and induces a new magnetic state due to the surface spins which is realized as diluted antiferromagnet in a field (DAFF) as explored by the thermoremanent and isothermoremanent magnetization measured with different applied magnetic field.

Green synthesis of gold nanoparticles using aqueous extract of Dillenia indica

NASA Astrophysics Data System (ADS)

Sett, Arghya; Gadewar, Manoj; Sharma, Pragya; Deka, Manab; Bora, Utpal

2016-06-01

In this study, we report a novel method of gold nanoparticle (AuNP) synthesis using aqueous fruit extract of Dillenia indica. The phytochemicals present in the fruit extract act as an effective reducing and capping agent to synthesize AuNPs. The synthesized AuNPs were characterized by spectrophotometry, transmission electron microscopy (TEM), x-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. TEM studies revealed the particles of various sizes and mainly spherical in shape. Selected-area electron diffraction (SAED) patterns and high-resolution transmission electron microscopy (HRTEM) images confirmed the crystallinity of the particles. The XRD patterns showed peaks at (111), (200), (220) which exhibited preferential orientation of the AuNPs as face-centered cubic crystal. FTIR measurements confirmed the coating of phenolic compounds on the AuNPs indicating a possible role of biomolecules for the capping and efficient stabilization of the AuNPs. The synthesized AuNPs did not show any form of cytotoxicity in the normal fibroblast cell line L929.

Structures and standard molar enthalpies of formation of a series of Ln(III)–Cu(II) heteronuclear compounds with pyrazine-2,3-dicarboxylic acid

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

Yang, Qi; Xie, Gang; Wei, Qing

2014-07-01

Fifteen lanthanide–copper heteronuclear compounds, formulated as [CuLn{sub 2}(pzdc){sub 4}(H{sub 2}O){sub 6}]·xH{sub 2}O (1–6(x=2), 8(x=3), 9–10(x=4)); [CuLn{sub 2}(pzdc){sub 4}(H{sub 2}O){sub 4}]·xH{sub 2}O (7, 12–13, 15(x=4), 14(x=5), 11(x=8)) (Ln(III)=La(1); Ce(2); Pr(3); Nd(4); Sm(5); Eu(6); Gd(7); Tb(8); Dy(9); Ho(10); Er(11); Tm(12); Yb(13); Lu(14); Y(15); H{sub 2}pzdc (C{sub 6}H{sub 4}N{sub 2}O{sub 4})=pyrazine-2,3-dicarboxylic acid) have been hydrothermally synthesized. All compounds were characterized by element analysis, IR spectroscopy, single-crystal X-ray diffraction and thermal analysis. X-ray diffraction analyses confirm that all compounds are isostructural and feature a 3D brick-like framework structure with (4.6{sup 2}){sub 2}(4{sup 2}.6{sup 2}.8{sup 2})(6{sup 3}){sup 2}(6{sup 5}.8){sub 2} topology. Using 1 mol cm{supmore » −3} HCl(aq) as calorimetric solvent, with an isoperibol solution–reaction calorimeter, the standard molar enthalpies of formation of all compounds were determined by a designed thermochemical cycle. In addition, solid state luminescence properties of compounds 5, 6, 8 and 9 were studied in the solid state. - Graphical abstract: According to Hess' rule, the standard molar enthalpies of formation of Ln–Cu heterometallic coordination compounds were determined by a designed thermochemical cycle. - Highlights: • Fifteen lanthanide–copper heteronuclear isostructural compounds. • Structurally characterization by IR, X-ray diffraction and thermal analysis. • The standard molar enthalpy of formation. • Isoperibol solution–reaction calorimetry.« less

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

Azmi, M. A.; Ismail, N. A. A.; Rizamarhaiza, M.

Rice husk was thermally decomposed to yield powder composed of silica (SiO{sub 2}). Temperatures of 700°C and 1000°C were chosen as the decomposition temperatures. X-Ray Diffraction (XRD), X-Ray Florescence (XRF), Fourier Transform Infrared (FTIR), and Field Emission Scanning Electron Microscope (FESEM) analyses were conducted on a synthetic silica powder (SS-SiO{sub 2}) and the rice husk ash as for the comparative characterisation study. XRD analyses clearly indicated that the decomposed rice husk yielded silica of different nature which are Crystalline Rice Husk Silica (C-RHSiO{sub 2}) and Amorphous Rice Husk Silica (A-RHSiO{sub 2}). Moreover, it was found that SS-SiO{sub 2} was ofmore » Quartz phase, C-RHSiO{sub 2} was of Trydimite and Cristobalite. Through XRF detection, the highest SiO{sub 2} purity was detected in SS-SiO{sub 2} followed by C-RHSiO{sub 2} and A-RHSiO{sub 2} with purity percentages of 99.60%, 82.30% and 86.30% respectively. FTIR results clearly indicated silica (SiO{sub 2}) bonding 1056, 1064, 1047, 777, 790 and 798 cm{sup −1}) increased as the crystallinity silica increased. The Cristobalite phase was detected in C-RH SiO{sub 2} at the wavelength of 620 cm{sup −1}. Morphological features as observed by FESEM analyses confirmed that, SS-SiO{sub 2} and C-RH SiO{sub 2} showed prominent coarse granular morphology.« less

Quantification of local strain distributions in nanoscale strained SiGe FinFET structures

NASA Astrophysics Data System (ADS)

Mochizuki, Shogo; Murray, Conal E.; Madan, Anita; Pinto, Teresa; Wang, Yun-Yu; Li, Juntao; Weng, Weihao; Jagannathan, Hemanth; Imai, Yasuhiko; Kimura, Shigeru; Takeuchi, Shotaro; Sakai, Akira

2017-10-01

Strain within nanoscale strained SiGe FinFET structures has been investigated using a combination of X-ray diffraction and transmission electron microscopy-based nanobeam diffraction (NBD) techniques to reveal the evolution of the stress state within the FinFETs. Reciprocal space maps collected using high-resolution X-ray diffraction exhibited distinct features corresponding to the SiGe fin width, pitch, and lattice deformation and were analyzed to quantify the state of stress within the fins. Although the majority of the SiGe fin volume exhibited a uniaxial stress state due to elastic relaxation of the transverse in-plane stress, NBD measurements confirmed a small interaction region near the SOI interface that is mechanically constrained by the underlying substrate. We have quantitatively characterized the evolution of the fin stress state from biaxial to uniaxial as a function of fin aspect ratio and Ge fraction and confirmed that the fins obey elastic deformation based on a model that depends on the relative difference between the equilibrium Si and SiGe lattice constants and relative fraction of in-plane stress transverse to the SiGe fins. Spatially resolved, nanobeam X-ray diffraction measurements conducted near the SiGe fin edge indicate the presence of additional elastic relaxation from a uniaxial stress state to a fully relaxed state at the fin edge. Mapping of the lattice deformation within 500 nm of this fin edge by NBD revealed large gradients, particularly at the top corner of the fin. The values of the volume averaged lattice deformation obtained by nanoXRD and NBD are qualitatively consistent. Furthermore, the modulation of strain at the fin edge obtained by quantitative analysis of the nanoXRD results agrees with the lattice deformation profile obtained by NBD.

A Medipix quantum area detector allows rotation electron diffraction data collection from submicrometre three-dimensional protein crystals

PubMed Central

Nederlof, Igor; van Genderen, Eric; Li, Yao-Wang; Abrahams, Jan Pieter

2013-01-01

When protein crystals are submicrometre-sized, X-ray radiation damage precludes conventional diffraction data collection. For crystals that are of the order of 100 nm in size, at best only single-shot diffraction patterns can be collected and rotation data collection has not been possible, irrespective of the diffraction technique used. Here, it is shown that at a very low electron dose (at most 0.1 e− Å−2), a Medipix2 quantum area detector is sufficiently sensitive to allow the collection of a 30-frame rotation series of 200 keV electron-diffraction data from a single ∼100 nm thick protein crystal. A highly parallel 200 keV electron beam (λ = 0.025 Å) allowed observation of the curvature of the Ewald sphere at low resolution, indicating a combined mosaic spread/beam divergence of at most 0.4°. This result shows that volumes of crystal with low mosaicity can be pinpointed in electron diffraction. It is also shown that strategies and data-analysis software (MOSFLM and SCALA) from X-ray protein crystallography can be used in principle for analysing electron-diffraction data from three-dimensional nanocrystals of proteins. PMID:23793148

Analysis and Correction of Diffraction Effect on the B/A Measurement at High Frequencies

NASA Astrophysics Data System (ADS)

Zhang, Dong; Gong, Xiu-Fen; Liu, Xiao-Zhou; Kushibiki, Jun-ichi; Nishino, Hideo

2004-01-01

A numerical method is developed to analyse and to correct the diffraction effect in the measurement of acoustic nonlinearity parameter B/A at high frequencies. By using the KZK nonlinear equation and the superposition approach of Gaussian beams, an analytical model is derived to describe the second harmonic generation through multi-layer medium SiO2/liquid specimen/SiO2. Frequency dependence of the nonlinear characterization curve for water in 110-155 MHz is numerically and experimentally investigated. With the measured dip position and the new model, values of B/A for water are evaluated. The results show that the present method can effectively correct the diffraction effect in the measurement.

How to make deposition of images a reality

PubMed Central

Guss, J. Mitchell; McMahon, Brian

2014-01-01

The IUCr Diffraction Data Deposition Working Group is investigating the rationale and policies for routine deposition of diffraction images (and other primary experimental data sets). An information-management framework is described that should inform policy directions, and some of the technical and other issues that need to be addressed in an effort to achieve such a goal are analysed. In the near future, routine data deposition could be encouraged at one of the growing number of institutional repositories that accept data sets or at a generic data-publishing web repository service. To realise all of the potential benefits of depositing diffraction data, specialized archives would be preferable. Funding such an initiative will be challenging. PMID:25286838

Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

DOE PAGES

Wang, H.; Kirkham, M. J.; Watkins, T. R.; ...

2016-02-17

N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« less

Auger electron diffraction study of Fe 1- xNi x alloys epitaxially grown on Cu(100)

NASA Astrophysics Data System (ADS)

Martin, M. G.; Foy, E.; Chevrier, F.; Krill, G.; Asensio, M. C.

1999-08-01

We have combined Auger electron diffraction (AED), low-energy electron diffraction (LEED) and high-energy electron diffraction (RHEED) to examine the structure of Fe xNi 1- x alloys when the Fe content approaches 65%. At this concentration, the 'invar effect' takes place, so the magnetization falls to zero, and the thermal expansion coefficient is very small. The Fe xNi 1- x alloys, grown as metastable thin films by molecular-beam epitaxy on Cu(100) substrates, were studied as a function of the x stoichiometry. In contrast to the related bulk alloy compounds, we observe the collapse of the fcc-to-bcc structural transition in the Fe-rich films. Furthermore, the local atomic structure around Fe and Ni in the alloy has been simultaneously determined by the angular intensity distributions of Fe L 3VV (703 eV) and Ni L 3VV (848 eV) Auger electrons measured as a function of polar and azimuthal angles. For the films deposited at room temperature, we have confirmed the pseudomorphic growth morphology and the uniformity of the alloys.

Electron diffraction study of the sillenites Bi{sub 12}SiO{sub 20}, Bi{sub 25}FeO{sub 39} and Bi{sub 25}InO{sub 39}: Evidence of short-range ordering of oxygen-vacancies in the trivalent sillenites

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

Scurti, Craig A.; Arenas, D. J.; Auvray, Nicolas

We present an electron diffraction study of three sillenites, Bi{sub 12}SiO{sub 20}, Bi{sub 25}FeO{sub 39}, and Bi{sub 25}InO{sub 39} synthesized using the solid-state method. We explore a hypothesis, inspired by optical studies in the literature, that suggests that trivalent sillenites have additional disorder not present in the tetravalent compounds. Electron diffraction patterns of Bi{sub 25}FeO{sub 39} and Bi{sub 25}InO{sub 39} show streaks that confirm deviations from the ideal sillenite structure. Multi-slice simulations of electron-diffraction patterns are presented for different perturbations to the sillenite structure - partial substitution of the M site by Bi{sup 3+}, random and ordered oxygen-vacancies, and amore » frozen-phonon model. Although comparison of experimental data to simulations cannot be conclusive, we consider the streaks as evidence of short-range ordered oxygen-vacancies.« less

Efficiency of a multilayer-Laue-lens with a 102 μm aperture

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

Macrander, Albert T., E-mail: atm@anl.gov; Wojcik, Michael; Maser, Jorg

2015-08-24

A multilayer-Laue-lens (MLL) comprised of WSi{sub 2}/Al layers stacked to a full thickness of 102 μm was characterized for its diffraction efficiency and dynamical diffraction properties by x-ray measurements made in the far field. The achieved aperture roughly doubles the previous maximum reported aperture for an MLL, thereby doubling the working distance. Negative and positive first orders were found to have 14.2% and 13.0% efficiencies, respectively. A section thickness of 9.6 μm was determined from Laue-case thickness fringes in the diffraction data. A background gas consisting of 90% Ar and 10% N{sub 2} was used for sputtering. This material system wasmore » chosen to reduce grown-in stress as the multilayer is deposited. Although some regions of the full MLL exhibited defects, the presently reported results were obtained for a region devoid of defects. The data compare well to dynamical diffraction calculations with Coupled Wave Theory (CWT) which provided confirmation of the optical constants and densities assumed for the CWT calculations.« less

Efficiency of a multilayer-Laue-lens with a 102 μm aperture

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

Macrander, Albert T.; Kubec, Adam; Conley, Raymond

2015-08-25

A multilayer-Laue-lens (MLL) comprised of WSi 2/Al layers stacked to a full thickness of 102 microns was characterized for its diffraction efficiency and dynamical diffraction properties by x-ray measurements made in the far field. The achieved aperture roughly doubles the previous maximum reported aperture for an MLL, thereby doubling the working distance. Negative and positive first orders were found to have 14.2 % and 13.0 % efficiencies, respectively. A section thickness of 9.6 μm was determined from Laue-case thickness fringes in the diffraction data. A background gas consisting of 90 % Ar and 10 % N 2 was used formore » sputtering. This material system was chosen to reduce grown-in stress as the multilayer is deposited. Although some regions of the full MLL exhibited defects, the presently reported results were obtained for a region devoid of defects. The data compare well to dynamical diffraction calculations with Coupled Wave Theory (CWT) which provided confirmation of the optical constants and densities assumed for the CWT calculations.« less

The strong ground motion in Mexico City: array and borehole data analysis.

NASA Astrophysics Data System (ADS)

Roullé, A.; Chávez-García, F. J.

2003-04-01

Site response at Mexico City has been intensively studied for the last 15 years, since the disastrous 1985 earthquakes. After those events, more than 100 accelerographs were installed, and their data have been extremely useful in quantifying amplification and in the subsequent upgrading of the building code. However, detailed analysis of the wavefield has been hampered by the lack of absolute time in the records and the large spacing between stations in terms of dominant wavelengths. In 2001, thanks to the support of CONACYT, Mexico, a new dense accelerographic network was installed in the lake bed zone of Mexico City. The entire network, including an existing network of 3 surface and 2 borehole stations operated by CENAPRED, consists in 12 surface and 4 borehole stations (at 30, 102 and 50 meters). Each station has a 18 bits recorder and a GPS receiver so that the complete network is a 3D array with absolute time. The main objective of this array is to provide data that can help us to better understand the wavefield that propagates in Mexico City during large earthquakes. Last year, a small event of magnitude 6.0 was partially recorded by 6 of the 12 surface stations and all the borehole stations. We analysed the surface data using different array processing techniques such as f-k methods and MUSIC algorithm and the borehole ones using a cross-correlation method. For periods inferior to the site resonance period, the soft clay layer with very low propagation velocities (less than 500 m/s) and a possible multipathing rule the wavefield pattern. For the large period range, the dominant surface wave comes from the epicentral direction and propagates with a quicker velocity (more than 1500 m/s) that corresponds to the velocity of deep layers. The analysis of borehole data shows the presence of different quick wavetrains in the short period range that could correspond to the first harmonic modes of Rayleigh waves. To complete this study, four others events recorded in 1994 by a temporal dense network installed in the firm rock zone of Mexico City were analysed using the same techniques. The results confirm the presence of a diffracting zone south of the valley. These results confirm the hypothesis of a possible interaction between the soft clay layers resonance and diffracted wavetrains of Rayleigh waves to explain both the amplification and the long duration of strong ground motion in Mexico City.

Synthesis of Novel Ferrite Based Recyclable Catalyst Used to Clean Dye and Emerging Contaminates from Water

EPA Science Inventory

Herein, we describe synthesis of novel palladium, copper, cobalt and vanadium ferrites. The ferrites were synthesized by combustion method using polyvinyl alcohol. The particles phases were confirmed using X-ray diffraction and sizes were determined using particle size analyzer. ...

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

Sathyalakshmi, R.; Bhagavannarayana, G.; Ramasamy, P.

L-(+)-Glutamic acid hydro bromide, an isomorphic salt of L-glutamic acid hydrochloride, was synthesized and the synthesis was confirmed using Fourier transform infrared analysis. Solubility of the material in water was determined. L-Glutamic acid hydro bromide crystals were grown by low temperature solution growth using the solvent evaporation technique. Single crystal X-ray diffraction studies were carried out and the cell parameters, atomic co-ordinates, bond lengths and bond angles were reported. High-resolution X-ray diffraction studies were carried out and good crystallinity for the grown crystal was observed from the diffraction curve. The grown crystals were subjected to dielectric studies. Ultraviolet-visible-near infrared spectralmore » analysis shows good optical transmission in the visible and infrared region of the grown crystals. The second harmonic generation efficiency of L-glutamic acid hydro bromide crystal was determined using the Kurtz powder test and it was found that it had efficiency comparable with that of the potassium di-hydrogen phosphate crystal.« less

Use of reciprocal lattice layer spacing in electron backscatter diffraction pattern analysis

PubMed

Michael; Eades

2000-03-01

In the scanning electron microscope using electron backscattered diffraction, it is possible to measure the spacing of the layers in the reciprocal lattice. These values are of great use in confirming the identification of phases. The technique derives the layer spacing from the higher-order Laue zone rings which appear in patterns from many materials. The method adapts results from convergent-beam electron diffraction in the transmission electron microscope. For many materials the measured layer spacing compares well with the calculated layer spacing. A noted exception is for higher atomic number materials. In these cases an extrapolation procedure is described that requires layer spacing measurements at a range of accelerating voltages. This procedure is shown to improve the accuracy of the technique significantly. The application of layer spacing measurements in EBSD is shown to be of use for the analysis of two polytypes of SiC.

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

Controlled nucleation and growth of CdS nanoparticles in a polymer matrix.

PubMed

Di Luccio, Tiziana; Laera, Anna Maria; Tapfer, Leander; Kempter, Susanne; Kraus, Robert; Nickel, Bert

2006-06-29

In-situ synchrotron X-ray diffraction (XRD) was used to monitor the thermal decomposition (thermolysis) of Cd thiolates precursors embedded in a polymer matrix and the nucleation of CdS nanoparticles. A thiolate precursor/polymer solid foil was heated to 300 degrees C in the X-ray diffraction setup of beamline W1.1 at Hasylab, and the diffraction curves were each recorded at 10 degrees C. At temperatures above 240 degrees C, the precursor decomposition is complete and CdS nanoparticles grow within the polymer matrix forming a nanocomposite with interesting optical properties. The nanoparticle structural properties (size and crystal structure) depend on the annealing temperature. Transmission electron microscopy (TEM) and photoluminescence (PL) analyses were used to characterize the nanoparticles. A possible mechanism driving the structural transformation of the precursor is inferred from the diffraction features arising at the different temperatures.

Nanoscale monoclinic domains in epitaxial SrRuO{sub 3} thin films deposited by pulsed laser deposition

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

Ghica, C., E-mail: cghica@infim.ro; Negrea, R. F.; Nistor, L. C.

2014-07-14

In this paper, we analyze the structural distortions observed by transmission electron microscopy in thin epitaxial SrRuO{sub 3} layers used as bottom electrodes in multiferroic coatings onto SrTiO{sub 3} substrates for future multiferroic devices. Regardless of the nature and architecture of the multilayer oxides deposited on the top of the SrRuO{sub 3} thin films, selected area electron diffraction patterns systematically revealed the presence of faint diffraction spots appearing in forbidden positions for the SrRuO{sub 3} orthorhombic structure. High-resolution transmission electron microscopy (HRTEM) combined with Geometric Phase Analysis (GPA) evidenced the origin of these forbidden diffraction spots in the presence ofmore » structurally disordered nanometric domains in the SrRuO{sub 3} bottom layers, resulting from a strain-driven phase transformation. The local high compressive strain (−4% ÷ −5%) measured by GPA in the HRTEM images induces a local orthorhombic to monoclinic phase transition by a cooperative rotation of the RuO{sub 6} octahedra. A further confirmation of the origin of the forbidden diffraction spots comes from the simulated diffraction patterns obtained from a monoclinic disordered SrRuO{sub 3} structure.« less

Empirically testing vaterite structural models using neutron diffraction and thermal analysis

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

Chakoumakos, Bryan C.; Pracheil, Brenda M.; Koenigs, Ryan

Otoliths, calcium carbonate (CaCO 3) ear bones, are among the most commonly used age and growth structures of fishes. Most fish otoliths are comprised of the most dense CaCO 3 polymorph, aragonite. Sturgeon otoliths, in contrast, have been characterized as the rare and structurally enigmatic polymorph, vaterite a metastable polymorph of CaCO 3. Vaterite is an important material ranging from biomedical to personal care applications although its crystal structure is highly debated. We characterized the structure of sturgeon otoliths using thermal analysis and neutron powder diffraction, which is used non-destructively. We confirmed that while sturgeon otoliths are primarily composed ofmore » vaterite, they also contain the denser CaCO 3 polymorph, calcite. For the vaterite fraction, neutron diffraction data provide enhanced discrimination of the carbonate group compared to x-ray diffraction data, owing to the different relative neutron scattering lengths, and thus offer the opportunity to uniquely test the more than one dozen crystal structural models that have been proposed for vaterite. Of those, space group P6 522 model, a = 7.1443(4)Å , c = 25.350(4)Å , V = 1121.5(2)Å 3 provides the best fit to the neutron powder diffraction data, and allows for a structure refinement using rigid carbonate groups.« less

Quantitative Imaging of Single Unstained Magnetotactic Bacteria by Coherent X-ray Diffraction Microscopy.

PubMed

Fan, Jiadong; Sun, Zhibin; Zhang, Jian; Huang, Qingjie; Yao, Shengkun; Zong, Yunbing; Kohmura, Yoshiki; Ishikawa, Tetsuya; Liu, Hong; Jiang, Huaidong

2015-06-16

Novel coherent diffraction microscopy provides a powerful lensless imaging method to obtain a better understanding of the microorganism at the nanoscale. Here we demonstrated quantitative imaging of intact unstained magnetotactic bacteria using coherent X-ray diffraction microscopy combined with an iterative phase retrieval algorithm. Although the signal-to-noise ratio of the X-ray diffraction pattern from single magnetotactic bacterium is weak due to low-scattering ability of biomaterials, an 18.6 nm half-period resolution of reconstructed image was achieved by using a hybrid input-output phase retrieval algorithm. On the basis of the quantitative reconstructed images, the morphology and some intracellular structures, such as nucleoid, polyβ-hydroxybutyrate granules, and magnetosomes, were identified, which were also confirmed by scanning electron microscopy and energy dispersive spectroscopy. With the benefit from the quantifiability of coherent diffraction imaging, for the first time to our knowledge, an average density of magnetotactic bacteria was calculated to be ∼1.19 g/cm(3). This technique has a wide range of applications, especially in quantitative imaging of low-scattering biomaterials and multicomponent materials at nanoscale resolution. Combined with the cryogenic technique or X-ray free electron lasers, the method could image cells in a hydrated condition, which helps to maintain their natural structure.

Empirically testing vaterite structural models using neutron diffraction and thermal analysis

DOE PAGES

Chakoumakos, Bryan C.; Pracheil, Brenda M.; Koenigs, Ryan; ...

2016-11-18

Otoliths, calcium carbonate (CaCO 3) ear bones, are among the most commonly used age and growth structures of fishes. Most fish otoliths are comprised of the most dense CaCO 3 polymorph, aragonite. Sturgeon otoliths, in contrast, have been characterized as the rare and structurally enigmatic polymorph, vaterite a metastable polymorph of CaCO 3. Vaterite is an important material ranging from biomedical to personal care applications although its crystal structure is highly debated. We characterized the structure of sturgeon otoliths using thermal analysis and neutron powder diffraction, which is used non-destructively. We confirmed that while sturgeon otoliths are primarily composed ofmore » vaterite, they also contain the denser CaCO 3 polymorph, calcite. For the vaterite fraction, neutron diffraction data provide enhanced discrimination of the carbonate group compared to x-ray diffraction data, owing to the different relative neutron scattering lengths, and thus offer the opportunity to uniquely test the more than one dozen crystal structural models that have been proposed for vaterite. Of those, space group P6 522 model, a = 7.1443(4)Å , c = 25.350(4)Å , V = 1121.5(2)Å 3 provides the best fit to the neutron powder diffraction data, and allows for a structure refinement using rigid carbonate groups.« less

Coriandrum sativum mediated synthesis of silver nanoparticles and evaluation of their biological characteristics

NASA Astrophysics Data System (ADS)

Senthilkumar, N.; Aravindhan, V.; Ruckmani, K.; Vetha Potheher, I.

2018-05-01

Silver (Ag) nanoparticles (NPs) were prepared by percolated green synthesis method using Coriandrum sativum leaf, root, seed and stem extracts and reported its antibacterial activity. The synthesized Ag NPs were confirmed by UV–visible Spectroscopy, Powder x-ray Diffraction (PXRD), Fourier Transform Infra Red (FT-IR) Spectroscopy analyzes. The Maximum absorbance observed around 400–450 nm reveal the characteristic absorbance of Ag NPs. The Dynamic Light Scattering (DLS) analysis shows the stability of synthesized NPs with average size varying from 35 to 53 nm and also zeta potential stability varying from ‑20 to ‑30 mV. The cubic structure, crystalline nature and purity of the material was confirmed by powder x-ray diffraction studies. FT-IR spectrum shows the presence of various functional groups in the resultant material. The Field Emission Scanning Electron Microscopy (FESEM) image shows the surface morphology of the synthesized NPs and the Energy Dispersive x-ray Analysis (EDAX) confirms the presence of silver metal ions. The Coriandrum sativum aqueous extract exhibited excellent antimicrobial activity against Klebsiella pneumoniae (Gram -ve) bacteria. Numerous studies have been made previously in our field of study but optimization has not been carried out by both extract (different parts like leaf, root, seed and stem) and without addition of any external source such as chemicals, heat etc.

Stereospecific growth of densely populated rutile mesoporous TiO2 nanoplate films: a facile low temperature chemical synthesis approach

NASA Astrophysics Data System (ADS)

Lee, Go-Woon; Ambade, Swapnil B.; Cho, Young-Jin; Mane, Rajaram S.; Shashikala, V.; Yadav, Jyotiprakash; Gaikwad, Rajendra S.; Lee, Soo-Hyoung; Jung, Kwang-Deog; Han, Sung-Hwan; Joo, Oh-Shim

2010-03-01

We report for the first time, using a simple and environmentally benign chemical method, the low temperature synthesis of densely populated upright-standing rutile TiO2 nanoplate films onto a glass substrate from a mixture of titanium trichloride, hydrogen peroxide and thiourea in triply distilled water. The rutile TiO2 nanoplate films (the phase is confirmed from x-ray diffraction analysis, selected area electron diffraction, energy-dispersive x-ray analysis, and Raman shift) are 20-35 nm wide and 100-120 nm long. The chemical reaction kinetics for the growth of these upright-standing TiO2 nanoplate films is also interpreted. Films of TiO2 nanoplates are optically transparent in the visible region with a sharp absorption edge close to 350 nm, confirming an indirect band gap energy of 3.12 eV. The Brunauer-Emmet-Teller surface area, Barret-Joyner-Halenda pore volume and pore diameter, obtained from N2 physisorption studies, are 82 m2 g - 1, 0.0964 cm3 g - 1 and 3.5 nm, respectively, confirming the mesoporosity of scratched rutile TiO2 nanoplate powder that would be ideal for the direct fabrication of nanoscaled devices including upcoming dye-sensitized solar cells and gas sensors.

Nd: YAG laser irradiation effects on structural and magnetic properties of Ni1+xZrxFe2-2xO4 nanoparticles

NASA Astrophysics Data System (ADS)

Saraf, Tukaram S.; Kounsalye, Jitendra S.; Birajdar, Shankar D.; Shamkuwar, N. R.

2018-05-01

The effect of 112 mJ Nd: YAG laser irradiation on structural, morphological, infrared and magnetic properties of Ni1+xZrxFe2-2xO4 spinel ferrite nanoparticles has been systematically investigated in the present work. The sol-gel auto combustion synthesis method was successfully executed for the synthesis of the present system. All the samples were characterized by X-ray diffraction technique (XRD), scanning electron microscopy (SEM) and infrared spectroscopy (IR) technique. The magnetic properties of the present samples were measured by pulse field hysteresis loop technique. All the properties were measured for laser irradiated samples as well, to understand the effect of irradiation on the properties. The single-phase cubic spinel structure was confirmed by X-ray diffraction patterns of all samples and the disordered structure was observed for irradiated samples. The two principle absorption bands in IR spectra also confirm the formation of the spinel structure. Spherical and agglomerated morphology was observed for Zr4+ substituted nickel ferrite, whereas scratched morphology was observed for the irradiated samples. The grain size confirms the nanocrystalline nature, the crystallite size also evident the same. The magnetic parameters decreased after Zr4+ ion doping and strongly influenced by the irradiation.

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

Holographic assembly of semiconductor CdSe quantum dots in polymer for volume Bragg grating structures with diffraction efficiency near 100%

NASA Astrophysics Data System (ADS)

Liu, Xiangming; Tomita, Yasuo; Oshima, Juro; Chikama, Katsumi; Matsubara, Koutatsu; Nakashima, Takuya; Kawai, Tsuyoshi

2009-12-01

We report on the fabrication of centimeter-size transmission Bragg gratings in semiconductor CdSe quantum dots dispersed 50 μm thick photopolymer films. This was done by holographic assembly of CdSe quantum dots in a photopolymerizable monomer blend. Periodic patterning of CdSe quantum dots in polymer was confirmed by a fluorescence microscope and confocal Raman imaging. The diffraction efficiency from the grating of 1 μm spacing was near 100% in the green with 0.34 vol % CdSe quantum dots, giving the refractive index modulation as large as 5.1×10-3.

Photoluminescence studies on Cd(1-x)Zn(x)S:Mn2+ nanocrystals.

PubMed

Sethi, Ruchi; Kumar, Lokendra; Pandey, A C

2009-09-01

Highly monodispersed, undoped and doped with Mn2+, binary and ternary (CdS, ZnS, Cd(1-x)Zn(x)S) compound semiconductor nanocrystals have been synthesized by co-precipitation method using citric acid as a stabilizer. As prepared sample are characterized by X-ray diffraction, Small angle X-ray scattering, Transmission electron microscope, Optical absorption and Photoluminescence spectroscopy, for their optical and structural properties. X-ray diffraction, Small angle X-ray scattering and Transmission electron microscope results confirm the preparation of monodispersed nanocrystals. Photoluminescence studies show a significant blue shift in the wavelength with an increasing concentration of Zn in alloy nanocrystals.

Synchronous scattering and diffraction from gold nanotextured surfaces with structure factors

NASA Astrophysics Data System (ADS)

Gu, Min-Jhong; Lee, Ming-Tsang; Huang, Chien-Hsun; Wu, Chi-Chun; Chen, Yu-Bin

2018-05-01

Synchronous scattering and diffraction were demonstrated using reflectance from gold nanotextured surfaces at oblique (θi = 15° and 60°) incidence of wavelength λ = 405 nm. Two samples of unique auto-correlation functions were cost-effectively fabricated. Multiple structure factors of their profiles were confirmed with Fourier expansions. Bi-directional reflectance function (BRDF) from these samples provided experimental proofs. On the other hand, standard deviation of height and unique auto-correlation function of each sample were used to generate surfaces numerically. Comparing their BRDF with those of totally random rough surfaces further suggested that structure factors in profile could reduce specular reflection more than totally random roughness.

Nanocrystalline NiNd0.01Fe1.99O4 as a gas sensor

NASA Astrophysics Data System (ADS)

Shinde, Tukaram J.; Gadkari, Ashok B.; Jadhav, Sarjerao R.; Kumar, Surender; Dalawai, Sanjeev P.; Vasambekar, Pramod N.

2015-06-01

Nanocrystalline NiNd0.01Fe1.99O4 has been synthesized by oxalate co-precipitation method and was characterized by X-ray diffraction technique. X-ray diffraction analysis confirms the formation of single phase cubic spinel structure. Crystallite size of the ferrite lies in the nano-particle range. The gas sensing properties of nanocrystalline ferrite were studied for gases like Cl2, LPG and C2H5OH. It was observed that NiNd0.01Fe1.99O4 is more sensitive towards chlorine followed by LPG at an operating temperature 277 °C compared to ethanol.

A protocol for searching the most probable phase-retrieved maps in coherent X-ray diffraction imaging by exploiting the relationship between convergence of the retrieved phase and success of calculation.

PubMed

Sekiguchi, Yuki; Hashimoto, Saki; Kobayashi, Amane; Oroguchi, Tomotaka; Nakasako, Masayoshi

2017-09-01

Coherent X-ray diffraction imaging (CXDI) is a technique for visualizing the structures of non-crystalline particles with size in the submicrometer to micrometer range in material sciences and biology. In the structural analysis of CXDI, the electron density map of a specimen particle projected along the direction of the incident X-rays can be reconstructed only from the diffraction pattern by using phase-retrieval (PR) algorithms. However, in practice, the reconstruction, relying entirely on the computational procedure, sometimes fails because diffraction patterns miss the data in small-angle regions owing to the beam stop and saturation of the detector pixels, and are modified by Poisson noise in X-ray detection. To date, X-ray free-electron lasers have allowed us to collect a large number of diffraction patterns within a short period of time. Therefore, the reconstruction of correct electron density maps is the bottleneck for efficiently conducting structure analyses of non-crystalline particles. To automatically address the correctness of retrieved electron density maps, a data analysis protocol to extract the most probable electron density maps from a set of maps retrieved from 1000 different random seeds for a single diffraction pattern is proposed. Through monitoring the variations of the phase values during PR calculations, the tendency for the PR calculations to succeed when the retrieved phase sets converged on a certain value was found. On the other hand, if the phase set was in persistent variation, the PR calculation tended to fail to yield the correct electron density map. To quantify this tendency, here a figure of merit for the variation of the phase values during PR calculation is introduced. In addition, a PR protocol to evaluate the similarity between a map of the highest figure of merit and other independently reconstructed maps is proposed. The protocol is implemented and practically examined in the structure analyses for diffraction patterns from aggregates of gold colloidal particles. Furthermore, the feasibility of the protocol in the structure analysis of organelles from biological cells is examined.

Remediation of uranium-contaminated groundwater by sorption onto hydoxyapatite derived from catfish bones

USDA-ARS?s Scientific Manuscript database

Hydroxyapatite was prepared from catfish bones, called catfish hydroxyapatite (CFHA), by mechanical and chemical treatment methods and was characterized by x-ray diffraction (X-RD) and scanning electron microscope (SEM) techniques to confirm the presence of hydroxyapatite. The ability of CFHA to rem...

Dielectric, electric and thermal properties of carboxylic functionalized multiwalled carbon nanotubes impregnated polydimethylsiloxane nanocomposite

NASA Astrophysics Data System (ADS)

Sagar, Sadia; Iqbal, Nadeem; Maqsood, Asghari

2013-06-01

The dielectric, electric and thermal properties of carboxylic functionalized multiwalled carbon nanotubes (F-MWCNT) incorporated into the polydimethylsiloxane (PDMS) were evaluated to determine their potential in the field of electronic materials. Carboxylic functionalization of the pristine multi walled carbon tubes (Ps-MWCNT) was confirmed through Fourier transform infrared spectroscopy, X-ray diffraction patterns for both Ps-MWCNTs and F-MWCNTs elaborated that crystalline behavior did not change with carboxylic moieties. Thermogravimetric and differential thermal analyses were performed to elucidate the thermal stability with increasing weight % addition of F-MWCNTs in the polymer matrix. Crystallization/glass transition / melting temperatures were evaluated using differential scanning calorimeter and it was observed that glass transition and crystallization temperatures were diminished while temperatures of first and second melting transitions were progressed with increasing F-MWCNT concentration in the PDMS matrix. Scanning electron microscopy and energy dispersive x-ray spectroscopy were carried out to confirm the morphology, functionalization, and uniform dispersion of F-MWCNTs in the polymer matrix. Electrical resistivity at temperature range (100-300°C), dielectric loss (tanδ) and dielectric parameters (epsilon/ epsilon//) were measured in the frequency range (1MHz-3GHz). The measured data simulate that the aforementioned properties were influenced by increasing filler contents in the polymer matrix because of the high polarization of conductive F-MWCNTs at the reinforcement/polymer interface.

Facile and fast synthesis of SnS2 nanoparticles by pulsed laser ablation in liquid

NASA Astrophysics Data System (ADS)

Johny, J.; Sepulveda-Guzman, S.; Krishnan, B.; Avellaneda, D.; Shaji, S.

2018-03-01

Nanoparticles (NPs) of tin disulfide (SnS2) were synthesized using pulsed laser ablation in liquid (PLAL) technique. Effects of different liquid media and ablation wavelengths on the morphology and optical properties of the nanoparticles were studied. Nd: YAG laser wavelengths of 532 nm and 1064 nm (frequency 10 Hz and pulse width 10 ns) were used to irradiate SnS2 target immersed in liquid for the synthesis of SnS2 nanoparticles. Here PLAL was a fast synthesis technique, the ablation was only for 30 s. Transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, UV-vis absorption spectroscopy and photoluminescence spectroscopy were used to characterize the SnS2 NPs. TEM images showed that the liquid medium and laser wavelength influence the morphology of the NPs. SAED patterns and high resolution TEM (HRTEM) images confirmed the crystallinity of the particles. XRD and XPS analyses confirmed that SnS2 NPs were having exact crystalline structure and chemical states as that of the target. Raman analysis also supported the results obtained by XRD and XPS. Optical band gaps of the nanocolloids evaluated from their UV-vis absorption spectra were 2.4-3.05 eV. SnS2 NPs were having luminescence spectra in the blue-green region irrespective of the liquid media and ablation wavelength.

Structural, thermal, laser damage, photoconductivity, NLO and mechanical properties of modified vertical Bridgman method grown AgGa0.5In0.5Se2 single crystal

NASA Astrophysics Data System (ADS)

Vijayakumar, P.; Ramasamy, P.

2016-08-01

AgGa0.5In0.5Se2 single crystal was grown using modified vertical Bridgman method. The structural perfection of the AgGa0.5In0.5Se2 single crystal has been analyzed by high-resolution X-ray diffraction rocking curve measurements. The structural and compositional uniformities of AgGa0.5In0.5Se2 were studied using Raman scattering spectroscopy at room temperature. The FWHM of the Γ1 (W1) and Γ5L (Γ15) measured at different regions of the crystal confirms that the composition throughout its length is fairly uniform. Thermal properties of the as-grown crystal, including specific heat, thermal diffusivity and thermal conductivity have been investigated. The multiple shot surface laser damage threshold value was measured using Nd:YAG laser. Photoconductivity measurements with different temperatures have confirmed the positive photoconducting behavior. Second harmonic generation (SHG) on powder samples has been measured using the Kurtz and Perry technique and the results display that AgGa0.5In0.5Se2 is a phase-matchable NLO material. The hardness behavior has been measured using Vickers micro hardness measurement and the indentation size effect has been observed. The classical Meyer's law, propositional resistance model and modified propositional resistance model have been used to analyse the micro hardness behavior.

Composited reduced graphene oxide into LiFePO4/Li2SiO3 and its electrochemical impedance spectroscopy properties

NASA Astrophysics Data System (ADS)

Arifin, M.; Rus, Y. B.; Aimon, A. H.; Iskandar, F.; Winata, T.; Abdullah, M.; Khairurrijal, K.

2017-03-01

LiFePO4 is commonly used as cathode material for Li-ion batteries due to its stable operational voltage and high specific capacity. However, it suffers from certain disadvantages such as low intrinsic electronic conductivity and low ionic diffusion. This study was conducted to analyse the effect of reduced graphene oxide (rGO) on the electrochemical properties of LiFePO4/Li2SiO3 composite. This composite was synthesized by a hydrothermal method. Fourier transform infrared spectroscopy measurement identified the O-P-O, Fe-O, P-O, and O-Si-O- bands in the LiFePO4/Li2SiO3 composite. X-ray diffraction measurement confirmed the formation of LiFePO4. Meanwhile, Raman spectroscopy confirmed the number of rGO layers. Further, scanning electron microscopy images showed that rGO was distributed around the LiFePO4/Li2SiO3 particles. Finally, the electrochemical impedance spectroscopy results showed that the addition of 1 wt% of rGO to the LiFePO4/Li2SiO3 composite reduced charge transfer resistance. It may be concluded that the addition of 1 wt% rGO to LiFePO4/Li2SiO3 composite can enhance its electrochemical performance as a cathode material.

Ziegler-Natta Catalyst Based on MgCl₂/Clay/ID/TiCl₄ for the Synthesis of Spherical Particles of Polypropylene Nanocomposites.

PubMed

Cardoso, Renata da Silva; Oliveira, Jaqueline da Silva; Ramis, Luciana Bortolin; Marques, Maria de Fátima V

2018-07-01

In the present work, we have designed MgCl2/clay/internal donor (ID)/TiCl4 based bisupported Ziegler-Natta catalysts containing varying amounts of organoclay (montmorillonite) in order to synthesize spherical particles of polypropylene/clay nanocomposites (PCN). The organoclay was introduced into the catalyst support formulation and PCN was obtained using the in situ polymerization technique. Decreasing the reaction time, it was possible to obtain nanocomposites with high concentrations of clay (masterbatches). Micrographs of SEM confirmed the spherical morphology of the catalysts. In addition, XRD patterns show that the active sites for polymerization were inserted in the clay galleries. The catalytic performance was evaluated in slurry propylene polymerization using triethylaluminium as cocatalyst and silane as external electron donor at 70 °C, 4 bar, and different reaction times. The PCNs obtained containing different clay amounts were characterized by X-ray diffraction, thermal analyses, transmission electronic microscopy, and extractables in heptane. The results revealed that the synthesized PP/clay particles were also spherical showing that the morphological control is possible even using catalysts containing high amounts of clay. The PCN presented high degradation temperature (459 °C). The XRD peak related to the clay interlamellar distance has shifted to lower angles, and TEM images confirmed the formation of exfoliated/intercalated clay on the PP matrix and absence of microparticles of clay.

Studies on the Fe3+ Doping Effect on Structural, Optical and Catalytic Properties of Hydrothermally Synthesized TiO2 Photocatalyst

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

Kamble, Ravi; Sabale, Sandip; Chikode, Prashant

2017-08-01

Pure TiO2 and Fe3+-TiO2 nanoparticles have been prepared by simple hydrothermal method with different Fe3+ concentrations. The synthesized nanoparticles are analysed to determine its structural, optical, morphological and compositional properties using X-ray diffraction, Raman, UV-DRS, photoluminescence, Mossbauer, XPS, TEM and SEM/EDS. The EDS micrograph confirms the existence of Fe3+ atoms in the TiO2 matrix with 0.85, 1.52 and 1.87 weight percent. The crystallite size and band gap decrease with increase in Fe3+concentration. The average particle size obtained from TEM is 7-11 nm which is in good agreement with XRD results. Raman bands at 640 cm-1, 517 cm-1 and 398 cm-1more » further confirm pure phase anatase in all samples. XPS shows the proper substitutions of few sites of Ti4+ ions by Fe3+ ions in the TiO2 host lattice. The intensity of PL spectra for Fe3+-TiO2 shows a gradual decrease in the peak intensity with increasing Fe3+ concentration in TiO2, and it indicates lower recombination rate as Fe3+ ions increases. These nanoparticles are further studied for its photocatalytic activities using malachite green dye under UV light, visible light and sunlight.« less

Immobilization of pectinase onto Fe3O4@SiO2-NH2 and its activity and stability.

PubMed

Fang, Gang; Chen, Honggao; Zhang, Yunpeng; Chen, Anqing

2016-07-01

Fe3O4 magnetic nanometer particles (MNPS) with a diameter of 30-40nm and coated by ammoniated silicon dioxides were developed by sol-gel method. The X-ray diffraction (XRD) pattern indicates that the Fe3O4 is wrapped in the amorphous SiO2, and the Fourier-transform infrared spectroscopy (FT-IR) analysis confirmed the NH2 group had been successfully introduced onto the surface of Fe3O4@SiO2 nanoparticles. The main factors related to the immobilization process of pectinase onto the magnetic support were optimized by multi-factor orthogonal experiments, and the recommended combination is that 3% glutaraldehyde (coupling agent), pH=8.0, 50°C, and cross-linking time 8h. Scanning electron microscope (SEM) and FT-IR analyses confirmed that the pectinase had been immobilized onto the surface of the amino modified nanoparticles. The storage stability and reusability of the pectinase were enhanced by the immobilization that 64.4% of the total starting activity was retrieved after 7 recycling batches and only about 21.1% of the total activity was lost after 30-day storage. For the application of the immobilized pectinase, the optimal pH and temperature were 8.5 and 55°C, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Spectral analysis of a family of binary inflation rules

NASA Astrophysics Data System (ADS)

Baake, Michael; Grimm, Uwe; Mañibo, Neil

2018-01-01

The family of primitive binary substitutions defined by 1 \\mapsto 0 \\mapsto 0 1^m with m\\in N is investigated. The spectral type of the corresponding diffraction measure is analysed for its geometric realisation with prototiles (intervals) of natural length. Apart from the well-known Fibonacci inflation (m=1 ), the inflation rules either have integer inflation factors, but non-constant length, or are of non-Pisot type. We show that all of them have singular diffraction, either of pure point type or essentially singular continuous.

Application of the fractional Fourier transformation to digital holography recorded by an elliptical, astigmatic Gaussian beam.

PubMed

Nicolas, F; Coëtmellec, S; Brunel, M; Allano, D; Lebrun, D; Janssen, A J E M

2005-11-01

The authors have studied the diffraction pattern produced by a particle field illuminated by an elliptic and astigmatic Gaussian beam. They demonstrate that the bidimensional fractional Fourier transformation is a mathematically suitable tool to analyse the diffraction pattern generated not only by a collimated plane wave [J. Opt. Soc. Am A 19, 1537 (2002)], but also by an elliptic and astigmatic Gaussian beam when two different fractional orders are considered. Simulations and experimental results are presented.

Rietveld Refinement on X-Ray Diffraction Patterns of Bioapatite in Human Fetal Bones

PubMed Central

Meneghini, Carlo; Dalconi, Maria Chiara; Nuzzo, Stefania; Mobilio, Settimio; Wenk, Rudy H.

2003-01-01

Bioapatite, the main constituent of mineralized tissue in mammalian bones, is a calcium-phosphate-based mineral that is similar in structure and composition to hydroxyapatite. In this work, the crystallographic structure of bioapatite in human fetuses was investigated by synchrotron radiation x-ray diffraction (XRD) and microdiffraction (μ-XRD) techniques. Rietveld refinement analyses of XRD and μ-XRD data allow for quantitative probing of the structural modifications of bioapatite as functions of the mineralization process and gestational age. PMID:12609904

Inorganic pyrophosphatase crystals from Thermococcus thioreducens for X-ray and neutron diffraction.

PubMed

Hughes, Ronny C; Coates, Leighton; Blakeley, Matthew P; Tomanicek, Steve J; Langan, Paul; Kovalevsky, Andrey Y; García-Ruiz, Juan M; Ng, Joseph D

2012-12-01

Inorganic pyrophosphatase (IPPase) from the archaeon Thermococcus thioreducens was cloned, overexpressed in Escherichia coli, purified and crystallized in restricted geometry, resulting in large crystal volumes exceeding 5 mm3. IPPase is thermally stable and is able to resist denaturation at temperatures above 348 K. Owing to the high temperature tolerance of the enzyme, the protein was amenable to room-temperature manipulation at the level of protein preparation, crystallization and X-ray and neutron diffraction analyses. A complete synchrotron X-ray diffraction data set to 1.85 Å resolution was collected at room temperature from a single crystal of IPPase (monoclinic space group C2, unit-cell parameters a=106.11, b=95.46, c=113.68 Å, α=γ=90.0, β=98.12°). As large-volume crystals of IPPase can be obtained, preliminary neutron diffraction tests were undertaken. Consequently, Laue diffraction images were obtained, with reflections observed to 2.1 Å resolution with I/σ(I) greater than 2.5. The preliminary crystallographic results reported here set in place future structure-function and mechanism studies of IPPase.

Structure determination of Ba5AlF13 by coupling electron, synchrotron and neutron powder diffraction, solid-state NMR and ab initio calculations.

PubMed

Martineau, Charlotte; Allix, Mathieu; Suchomel, Matthew R; Porcher, Florence; Vivet, François; Legein, Christophe; Body, Monique; Massiot, Dominique; Taulelle, Francis; Fayon, Franck

2016-10-04

The room temperature structure of Ba 5 AlF 13 has been investigated by coupling electron, synchrotron and neutron powder diffraction, solid-state high-resolution NMR ( 19 F and 27 Al) and first principles calculations. An initial structural model has been obtained from electron and synchrotron powder diffraction data, and its main features have been confirmed by one- and two-dimensional NMR measurements. However, DFT GIPAW calculations of the 19 F isotropic shieldings revealed an inaccurate location of one fluorine site (F3, site 8a), which exhibited unusual long F-Ba distances. The atomic arrangement was reinvestigated using neutron powder diffraction data. Subsequent Fourier maps showed that this fluorine atom occupies a crystallographic site of lower symmetry (32e) with partial occupancy (25%). GIPAW computations of the NMR parameters validate the refined structural model, ruling out the presence of local static disorder and indicating that the partial occupancy of this F site reflects a local motional process. Visualisation of the dynamic process was then obtained from the Rietveld refinement of neutron diffraction data using an anharmonic description of the displacement parameters to account for the thermal motion of the mobile fluorine. The whole ensemble of powder diffraction and NMR data, coupled with first principles calculations, allowed drawing an accurate structural model of Ba 5 AlF 13 , including site-specific dynamical disorder in the fluorine sub-network.

Characterization of cellulosic wastes and gasification products from chicken farms

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

Joseph, Paul, E-mail: p.joseph@ulster.ac.uk; Tretsiakova-McNally, Svetlana; McKenna, Siobhan

Highlights: Black-Right-Pointing-Pointer The gas chromatography indicated the variable quality of the producer gas. Black-Right-Pointing-Pointer The char had appreciable NPK values, and can be used as a fertiliser. Black-Right-Pointing-Pointer The bio-oil produced was of poor quality, having high moisture content and low pH. Black-Right-Pointing-Pointer Mass and energy balances showed inadequate level energy recovery from the process. Black-Right-Pointing-Pointer Future work includes changing the operating parameters of the gasification unit. - Abstract: The current article focuses on gasification as a primary disposal solution for cellulosic wastes derived from chicken farms, and the possibility to recover energy from this process. Wood shavings and chickenmore » litter were characterized with a view to establishing their thermal parameters, compositional natures and calorific values. The main products obtained from the gasification of chicken litter, namely, producer gas, bio-oil and char, were also analysed in order to establish their potential as energy sources. The experimental protocol included bomb calorimetry, pyrolysis combustion flow calorimetry (PCFC), thermo-gravimetric analyses (TGA), differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy, elemental analyses, X-ray diffraction (XRD), mineral content analyses and gas chromatography. The mass and energy balances of the gasification unit were also estimated. The results obtained confirmed that gasification is a viable method of chicken litter disposal. In addition to this, it is also possible to recover some energy from the process. However, energy content in the gas-phase was relatively low. This might be due to the low energy efficiency (19.6%) of the gasification unit, which could be improved by changing the operation parameters.« less

Exchangeable Ions Are Responsible for the In Vitro Antibacterial Properties of Natural Clay Mixtures

PubMed Central

Otto, Caitlin C.; Haydel, Shelley E.

2013-01-01

We have identified a natural clay mixture that exhibits in vitro antibacterial activity against a broad spectrum of bacterial pathogens. We collected four samples from the same source and demonstrated through antibacterial susceptibility testing that these clay mixtures have markedly different antibacterial activity against Escherichia coli and methicillin-resistant Staphylococcus aureus (MRSA). Here, we used X-ray diffraction (XRD) and inductively coupled plasma – optical emission spectroscopy (ICP-OES) and – mass spectrometry (ICP-MS) to characterize the mineralogical and chemical features of the four clay mixture samples. XRD analyses of the clay mixtures revealed minor mineralogical differences between the four samples. However, ICP analyses demonstrated that the concentrations of many elements, Fe, Co, Cu, Ni, and Zn, in particular, vary greatly across the four clay mixture leachates. Supplementation of a non-antibacterial leachate containing lower concentrations of Fe, Co, Ni, Cu, and Zn to final ion concentrations and a pH equivalent to that of the antibacterial leachate generated antibacterial activity against E. coli and MRSA, confirming the role of these ions in the antibacterial clay mixture leachates. Speciation modeling revealed increased concentrations of soluble Cu2+ and Fe2+ in the antibacterial leachates, compared to the non-antibacterial leachates, suggesting these ionic species specifically are modulating the antibacterial activity of the leachates. Finally, linear regression analyses comparing the log10 reduction in bacterial viability to the concentration of individual ion species revealed positive correlations with Zn2+ and Cu2+ and antibacterial activity, a negative correlation with Fe3+, and no correlation with pH. Together, these analyses further indicate that the ion concentration of specific species (Fe2+, Cu2+, and Zn2+) are responsible for antibacterial activity and that killing activity is not solely attributed to pH. PMID:23691149

An X-ray diffraction method for semiquantitative mineralogical analysis of Chilean nitrate ore

USGS Publications Warehouse

Jackson, J.C.; Ericksent, G.E.

1997-01-01

Computer analysis of X-ray diffraction (XRD) data provides a simple method for determining the semiquantitative mineralogical composition of naturally occurring mixtures of saline minerals. The method herein described was adapted from a computer program for the study of mixtures of naturally occurring clay minerals. The program evaluates the relative intensities of selected diagnostic peaks for the minerals in a given mixture, and then calculates the relative concentrations of these minerals. The method requires precise calibration of XRD data for the minerals to be studied and selection of diffraction peaks that minimize inter-compound interferences. The calculated relative abundances are sufficiently accurate for direct comparison with bulk chemical analyses of naturally occurring saline mineral assemblages.

An x-ray diffraction method for semiquantitative mineralogical analysis of chilean nitrate ore

USGS Publications Warehouse

John, C.; George, J.; Ericksen, E.

1997-01-01

Computer analysis of X-ray diffraction (XRD) data provides a simple method for determining the semiquantitative mineralogical composition of naturally occurring mixtures of saline minerals. The method herein described was adapted from a computer program for the study of mixtures of naturally occurring clay minerals. The program evaluates the relative intensities of selected diagnostic peaks for the minerals in a given mixture, and then calculates the relative concentrations of these minerals. The method requires precise calibration of XRD data for the minerals to be studied and selection of diffraction peaks that minimize inter-compound interferences. The calculated relative abundances are sufficiently accurate for direct comparison with bulk chemical analyses of naturally occurring saline mineral assemblages.

Proton irradiated graphite grades for a long baseline neutrino facility experiment

NASA Astrophysics Data System (ADS)

Simos, N.; Nocera, P.; Zhong, Z.; Zwaska, R.; Mokhov, N.; Misek, J.; Ammigan, K.; Hurh, P.; Kotsina, Z.

2017-07-01

In search of a low-Z pion production target for the Long Baseline Neutrino Facility (LBNF) of the Deep Underground Neutrino Experiment (DUNE) four graphite grades were irradiated with protons in the energy range of 140-180 MeV, to peak fluence of ˜6.1 ×1020 p /cm2 and irradiation temperatures between 120 - 200 °C . The test array included POCO ZXF-5Q, Toyo-Tanso IG 430, Carbone-Lorraine 2020 and SGL R7650 grades of graphite. Irradiation was performed at the Brookhaven Linear Isotope Producer. Postirradiation analyses were performed with the objective of (a) comparing their response under the postulated irradiation conditions to guide a graphite grade selection for use as a pion target and (b) understanding changes in physical and mechanical properties as well as microstructure that occurred as a result of the achieved fluence and in particular at this low-temperature regime where pion graphite targets are expected to operate. A further goal of the postirradiation evaluation was to establish a proton-neutron correlation damage on graphite that will allow for the use of a wealth of available neutron-based damage data in proton-based studies and applications. Macroscopic postirradiation analyses as well as energy dispersive x-ray diffraction of 200 KeV x rays at the NSLS synchrotron of Brookhaven National Laboratory were employed. The macroscopic analyses revealed differences in the physical and strength properties of the four grades with behavior however under proton irradiation that qualitatively agrees with that reported for graphite under neutrons for the same low temperature regime and in particular the increase of thermal expansion, strength and Young's modulus. The proton fluence level of ˜1020 cm-2 where strength reaches a maximum before it begins to decrease at higher fluences has been identified and it agrees with neutron-induced changes. X-ray diffraction analyses of the proton irradiated graphite revealed for the first time the similarity in microstructural graphite behavior to that under neutron irradiation and the agreement between the fluence threshold of ˜5 ×1020 cm-2 where the graphite lattice undergoes a dramatic change. The confirmed similarity in behavior and agreement in threshold fluences for proton and neutron irradiation effects on graphite reported for the first time in this study will enable the safe utilization of the wealth of neutron irradiation data on graphite that extends to much higher fluences and different temperature regimes by the proton accelerator community searching for multi-MW graphite targets.

Proton irradiated graphite grades for a long baseline neutrino facility experiment

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

Simos, N.; Nocera, P.; Zhong, Z.

In search of a low-Z pion production target for the Long Baseline Neutrino Facility (LBNF) of the Deep Underground Neutrino Experiment (DUNE) four graphite grades were irradiated with protons in the energy range of 140–180 MeV, to peak fluence of ~6.1×10 20 p/cm 2 and irradiation temperatures between 120–200 °C. The test array included POCO ZXF-5Q, Toyo-Tanso IG 430, Carbone-Lorraine 2020 and SGL R7650 grades of graphite. Irradiation was performed at the Brookhaven Linear Isotope Producer. Postirradiation analyses were performed with the objective of (a) comparing their response under the postulated irradiation conditions to guide a graphite grade selection for use asmore » a pion target and (b) understanding changes in physical and mechanical properties as well as microstructure that occurred as a result of the achieved fluence and in particular at this low-temperature regime where pion graphite targets are expected to operate. A further goal of the postirradiation evaluation was to establish a proton-neutron correlation damage on graphite that will allow for the use of a wealth of available neutron-based damage data in proton-based studies and applications. Macroscopic postirradiation analyses as well as energy dispersive x-ray diffraction of 200 KeV x rays at the NSLS synchrotron of Brookhaven National Laboratory were employed. The macroscopic analyses revealed differences in the physical and strength properties of the four grades with behavior however under proton irradiation that qualitatively agrees with that reported for graphite under neutrons for the same low temperature regime and in particular the increase of thermal expansion, strength and Young’s modulus. The proton fluence level of ~10 20 cm -2 where strength reaches a maximum before it begins to decrease at higher fluences has been identified and it agrees with neutron-induced changes. X-ray diffraction analyses of the proton irradiated graphite revealed for the first time the similarity in microstructural graphite behavior to that under neutron irradiation and the agreement between the fluence threshold of ~5×10 20 cm -2 where the graphite lattice undergoes a dramatic change. The confirmed similarity in behavior and agreement in threshold fluences for proton and neutron irradiation effects on graphite reported for the first time in this study will enable the safe utilization of the wealth of neutron irradiation data on graphite that extends to much higher fluences and different temperature regimes by the proton accelerator community searching for multi-MW graphite targets.« less

Proton irradiated graphite grades for a long baseline neutrino facility experiment

DOE PAGES

Simos, N.; Nocera, P.; Zhong, Z.; ...

2017-07-24

In search of a low-Z pion production target for the Long Baseline Neutrino Facility (LBNF) of the Deep Underground Neutrino Experiment (DUNE) four graphite grades were irradiated with protons in the energy range of 140–180 MeV, to peak fluence of ~6.1×10 20 p/cm 2 and irradiation temperatures between 120–200 °C. The test array included POCO ZXF-5Q, Toyo-Tanso IG 430, Carbone-Lorraine 2020 and SGL R7650 grades of graphite. Irradiation was performed at the Brookhaven Linear Isotope Producer. Postirradiation analyses were performed with the objective of (a) comparing their response under the postulated irradiation conditions to guide a graphite grade selection for use asmore » a pion target and (b) understanding changes in physical and mechanical properties as well as microstructure that occurred as a result of the achieved fluence and in particular at this low-temperature regime where pion graphite targets are expected to operate. A further goal of the postirradiation evaluation was to establish a proton-neutron correlation damage on graphite that will allow for the use of a wealth of available neutron-based damage data in proton-based studies and applications. Macroscopic postirradiation analyses as well as energy dispersive x-ray diffraction of 200 KeV x rays at the NSLS synchrotron of Brookhaven National Laboratory were employed. The macroscopic analyses revealed differences in the physical and strength properties of the four grades with behavior however under proton irradiation that qualitatively agrees with that reported for graphite under neutrons for the same low temperature regime and in particular the increase of thermal expansion, strength and Young’s modulus. The proton fluence level of ~10 20 cm -2 where strength reaches a maximum before it begins to decrease at higher fluences has been identified and it agrees with neutron-induced changes. X-ray diffraction analyses of the proton irradiated graphite revealed for the first time the similarity in microstructural graphite behavior to that under neutron irradiation and the agreement between the fluence threshold of ~5×10 20 cm -2 where the graphite lattice undergoes a dramatic change. The confirmed similarity in behavior and agreement in threshold fluences for proton and neutron irradiation effects on graphite reported for the first time in this study will enable the safe utilization of the wealth of neutron irradiation data on graphite that extends to much higher fluences and different temperature regimes by the proton accelerator community searching for multi-MW graphite targets.« less

Synthesis and properties of silver nanoparticles in sodium bismuth borate glasses

NASA Astrophysics Data System (ADS)

Patwari, D. Rajeshree; Eraiah, B.

2018-04-01

Rare earth doped Sodium Bismuth Borate glass samples with silver chloride were prepared by melt quenching method. X-Ray diffraction pattern was used to confirm the amorphous nature of the samples. UV-Visible Spectra was recorded to study the optical properties. Surface plasmon resonance (SPR) peak was observed due to the formation of silver nanoparticles before and after heat treatment and the presence of silver nanoparticles were confirmed by UV-Visible Spectral studies and transmission electron microscopy. The surface plasmon resonance band became wider and red shifted after longer heat treatment.

Growth and characterization of KDP crystals doped with L-aspartic acid.

PubMed

Krishnamurthy, R; Rajasekaran, R; Samuel, Bincy Susan

2013-03-01

Potassium Dihydrogen Phosphate (KDP) doped with L-aspartic acid has been grown by solvent slow evaporation technique from a mixture of aqueous solution of KDP and 0.7% of L-aspartic acid at room temperature. The grown crystals were characterized by powder X-ray diffraction, UV-visible, FTIR analysis. The doping of aspartic acid was confirmed by FTIR spectrum. The Nonlinear optical property (SHG) of L-aspartic acid doped KDP has been confirmed. Microhardness studies were carried out on the grown crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis, investigation and spectroscopic characterization of piroxicam ternary complexes of Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with glycine and DL-phenylalanine.

PubMed

Mohamed, Gehad G; El-Gamel, Nadia E A

2004-11-01

The ternary piroxicam (Pir; 4-hydroxy-2-methyl-N-(2-pyridyl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide) complexes of Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with various amino acids (AA) such as glycine (Gly) or DL-phenylalanine (PhA) were prepared and characterized by elemental analyses, molar conductance, IR, UV-Vis, magnetic moment, diffuse reflectance and X-ray powder diffraction. The UV-Vis spectra of Pir and the effect of metal chelation on the different interligand transitions are discussed in detailed manner. IR and UV-Vis spectra confirm that Pir behaves as a neutral bidentate ligand coordinated to the metal ions via the pyridine-N and carbonyl group of the amide moiety. Gly molecule acted as a uninegatively monodentate ligand and coordinate to the metal ions through its carboxylic group, in addition PhA acted as a uninegatively bidentate ligand and coordinate to the metal ions through its carboxylic and amino groups. All the chelates have octahedral geometrical structures while Cu(II)- and Zn(II)-ternary chelates with PhA have square planar geometrical structures. The molar conductance data reveal that most of these chelates are non electrolytes, while Fe(III)-Pir-Gly, Co(II)-, Ni(II)-, Cu(II)- and Zn(II)-Pir-PhA chelates were 1:1 electrolytes. X-ray powder diffraction is used as a new tool to estimate the crystallinity of chelates as well as to elucidate their geometrical structures.

Synthesis, investigation and spectroscopic characterization of piroxicam ternary complexes of Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with glycine and DL-phenylalanine

NASA Astrophysics Data System (ADS)

Mohamed, Gehad G.; El-Gamel, Nadia E. A.

2004-11-01

The ternary piroxicam (Pir; 4-hydroxy-2-methyl- N-(2-pyridyl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide) complexes of Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with various amino acids (AA) such as glycine (Gly) or DL-phenylalanine (PhA) were prepared and characterized by elemental analyses, molar conductance, IR, UV-Vis, magnetic moment, diffuse reflectance and X-ray powder diffraction. The UV-Vis spectra of Pir and the effect of metal chelation on the different interligand transitions are discussed in detailed manner. IR and UV-Vis spectra confirm that Pir behaves as a neutral bidentate ligand coordinated to the metal ions via the pyridine- N and carbonyl group of the amide moiety. Gly molecule acted as a uninegatively monodentate ligand and coordinate to the metal ions through its carboxylic group, in addition PhA acted as a uninegatively bidentate ligand and coordinate to the metal ions through its carboxylic and amino groups. All the chelates have octahedral geometrical structures while Cu(II)- and Zn(II)-ternary chelates with PhA have square planar geometrical structures. The molar conductance data reveal that most of these chelates are non electrolytes, while Fe(III)-Pir-Gly, Co(II)-, Ni(II)-, Cu(II)- and Zn(II)-Pir-PhA cheletes were 1:1 electrolytes. X-ray powder diffraction is used as a new tool to estimate the crystallinity of chelates as well as to elucidate their geometrical structures.

Topotactic Reactions, Structural Studies, and Lithium Intercalation in Cation-Deficient Spinels with Formula Close to Li 2Mn 4O 9

NASA Astrophysics Data System (ADS)

Palos, A. Ibarra; Anne, M.; Strobel, P.

2001-08-01

The composition Li2Mn4O9, reported as a spinel oxide containing vacancies on both tetrahedral and octahedral sites [A. de Kock et al., Mater. Res. Bull. 25, 657 (1990)], was approached using three different preparation routes: low-temperature solid state reaction (A), chemical delithiation (B), and electrochemical delithiation (C). Rietveld refinements from neutron diffraction data confirmed the double-vacancy scheme proposed previously for product A, but with more tetrahedral and fewer octahedral vacancies than in the ideal Li2Mn4O9 formula. Low-temperature solid state reactions systematically result in broad reflections. Sample B, which was obtained topotactically, exhibits much narrower reflections. But chemical analyses, thermogravimetry, and neutron diffraction show that the acid treatment introduces significant amounts of protons, resulting in a formula close to Li0.92HMn4O9. Samples A and B were cycled electrochemically in lithium cells at 3 V with better stability than LiMn2O4, probably due to their higher initial manganese oxidation state. No separate electrochemical step linked to the filling of vacancies is observed in A, whereas B gives an additional redox step ca. 200 mV above the main plateau. This feature is not observed on compounds A or C; it is reversible, and seems to be a specific property of this spinel with a low initial cell parameter (8.09 Å). Sample A2 with double cation vacancies is especially stable on cycling at 3 V, and shows a very small volume variation on lithium intercalation.

Evidence of multimicrometric coherent γ' precipitates in a hot-forged γ-γ' nickel-based superalloy.

PubMed

Charpagne, M-A; Vennéguès, P; Billot, T; Franchet, J-M; Bozzolo, N

2016-07-01

This paper demonstrates the existence of large γ' precipitates (several micrometres in diameter) that are coherent with their surrounding matrix grain in a commercial γ-γ' nickel-based superalloy. The use of combined energy dispersive X-ray spectrometry and electron backscattered diffraction (EBSD) analyses allowed for revealing that surprising feature, which was then confirmed by transmission electron microscopy (TEM). Coherency for such large second-phase particles is supported by a very low crystal lattice misfit between the two phases, which was confirmed thanks to X-ray diffractograms and TEM selected area electron diffraction patterns. Dynamic recrystallization of polycrystalline γ-γ' nickel-based superalloys has been extensively studied in terms of mechanisms and kinetics. As in many materials with low stacking fault energy, under forging conditions, the main softening mechanism is discontinuous dynamic recrystallization. This mechanism occurs with preferential nucleation on the grain boundaries of the deformed matrix. The latter is then being consumed by the growth of the newly formed grains of low energy and by nucleation that keeps generating new grains. In the case of sub-solvus forging, large γ' particles usually pin the migrating boundaries and thus limit grain growth to a size which is determined by the distribution of second-phase particles, in good agreement with the Smith-Zener model. Under particular circumstances, the driving force associated with the difference in stored energy between the growing grains and the matrix can be large enough that the pinning forces can be overcome, and some grains can then reach much larger grain sizes. In the latter exceptional case, some intragranular primary γ' particles can be observed, although they are almost exclusively located on grain boundaries and triple junctions otherwise. In both cases, primary precipitates have no special orientation relationship with the surrounding matrix grain(s). This paper demonstrates the existence of high fractions of large γ' precipitate (several micrometres in diameter) that are coherent with their surrounding matrix grain, in a commercial γ-γ' nickel-based superalloy. Such a configuration is very surprising, because there is apparently no reason for the coherency of such particles. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Swinging Symmetry, Multiple Structural Phase Transitions, and Versatile Physical Properties in RECuGa3 (RE = La-Nd, Sm-Gd).

PubMed

Subbarao, Udumula; Rayaprol, Sudhindra; Dally, Rebecca; Graf, Michael J; Peter, Sebastian C

2016-01-19

The compounds RECuGa3 (RE = La-Nd, Sm-Gd) were synthesized by various techniques. Preliminary X-ray diffraction (XRD) analyses at room temperature suggested that the compounds crystallize in the tetragonal system with either the centrosymmetric space group I4/mmm (BaAl4 type) or the non-centrosymmetric space group I4mm (BaNiSn3 type). Detailed single-crystal XRD, neutron diffraction, and synchrotron XRD studies of selected compounds confirmed the non-centrosymmetric BaNiSn3 structure type at room temperature with space group I4mm. Temperature-dependent single-crystal XRD, powder XRD, and synchrotron beamline measurements showed a structural transition between centro- and non-centrosymmetry followed by a phase transition to the Rb5Hg19 type (space group I4/m) above 400 K and another transition to the Cu3Au structure type (space group Pm3̅m) above 700 K. Combined single-crystal and synchrotron powder XRD studies of PrCuGa3 at high temperatures revealed structural transitions at higher temperatures, highlighting the closeness of the BaNiSn3 structure to other structure types not known to the RECuGa3 family. The crystal structure of RECuGa3 is composed of eight capped hexagonal prism cages [RE4Cu4Ga12] occupying one rare-earth atom in each ring, which are shared through the edge of Cu and Ga atoms along the ab plane, resulting in a three-dimensional network. Resistivity and magnetization measurements demonstrated that all of these compounds undergo magnetic ordering at temperatures between 1.8 and 80 K, apart from the Pr and La compounds: the former remains paramagnetic down to 0.3 K, while superconductivity was observed in the La compound at T = 1 K. It is not clear whether this is intrinsic or due to filamentary Ga present in the sample. The divalent nature of Eu in EuCuGa3 was confirmed by magnetization measurements and X-ray absorption near edge spectroscopy and is further supported by the crystal structure analysis.

Novel Perspectives on the Characterization of Species-Dependent Optical Signatures of Bacterial Colonies by Digital Holography.

PubMed

Buzalewicz, Igor; Kujawińska, Małgorzata; Krauze, Wojciech; Podbielska, Halina

2016-01-01

The use of light diffraction for the microbiological diagnosis of bacterial colonies was a significant breakthrough with widespread implications for the food industry and clinical practice. We previously confirmed that optical sensors for bacterial colony light diffraction can be used for bacterial identification. This paper is focused on the novel perspectives of this method based on digital in-line holography (DIH), which is able to reconstruct the amplitude and phase properties of examined objects, as well as the amplitude and phase patterns of the optical field scattered/diffracted by the bacterial colony in any chosen observation plane behind the object from single digital hologram. Analysis of the amplitude and phase patterns inside a colony revealed its unique optical properties, which are associated with the internal structure and geometry of the bacterial colony. Moreover, on a computational level, it is possible to select the desired scattered/diffracted pattern within the entire observation volume that exhibits the largest amount of unique, differentiating bacterial features. These properties distinguish this method from the already proposed sensing techniques based on light diffraction/scattering of bacterial colonies. The reconstructed diffraction patterns have a similar spatial distribution as the recorded Fresnel patterns, previously applied for bacterial identification with over 98% accuracy, but they are characterized by both intensity and phase distributions. Our results using digital holography provide new optical discriminators of bacterial species revealed in one single step in form of new optical signatures of bacterial colonies: digital holograms, reconstructed amplitude and phase patterns, as well as diffraction patterns from all observation space, which exhibit species-dependent features. To the best of our knowledge, this is the first report on bacterial colony analysis via digital holography and our study represents an innovative approach to the subject.

Novel Perspectives on the Characterization of Species-Dependent Optical Signatures of Bacterial Colonies by Digital Holography

PubMed Central

Buzalewicz, Igor; Kujawińska, Małgorzata; Krauze, Wojciech; Podbielska, Halina

2016-01-01

The use of light diffraction for the microbiological diagnosis of bacterial colonies was a significant breakthrough with widespread implications for the food industry and clinical practice. We previously confirmed that optical sensors for bacterial colony light diffraction can be used for bacterial identification. This paper is focused on the novel perspectives of this method based on digital in-line holography (DIH), which is able to reconstruct the amplitude and phase properties of examined objects, as well as the amplitude and phase patterns of the optical field scattered/diffracted by the bacterial colony in any chosen observation plane behind the object from single digital hologram. Analysis of the amplitude and phase patterns inside a colony revealed its unique optical properties, which are associated with the internal structure and geometry of the bacterial colony. Moreover, on a computational level, it is possible to select the desired scattered/diffracted pattern within the entire observation volume that exhibits the largest amount of unique, differentiating bacterial features. These properties distinguish this method from the already proposed sensing techniques based on light diffraction/scattering of bacterial colonies. The reconstructed diffraction patterns have a similar spatial distribution as the recorded Fresnel patterns, previously applied for bacterial identification with over 98% accuracy, but they are characterized by both intensity and phase distributions. Our results using digital holography provide new optical discriminators of bacterial species revealed in one single step in form of new optical signatures of bacterial colonies: digital holograms, reconstructed amplitude and phase patterns, as well as diffraction patterns from all observation space, which exhibit species-dependent features. To the best of our knowledge, this is the first report on bacterial colony analysis via digital holography and our study represents an innovative approach to the subject. PMID:26943121

Study of structural and optical properties of YAG and Nd:YAG single crystals

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

Kostić, S.; Lazarević, Z.Ž., E-mail: lzorica@yahoo.com; Radojević, V.

2015-03-15

Highlights: • Transparent YAG and pale pink Nd:YAG single crystals were produced by the Czochralski technique. • Growth mechanisms and shape of the liquid/solid interface and incorporation of Nd{sup 3+} were studied. • The structure of the crystals was investigated by X-ray diffraction, Raman and IR spectroscopy. • The 15 Raman and 17 IR modes were observed. • The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. - Abstract: Yttrium aluminum garnet (YAG, Y{sub 3}Al{sub 5}O{sub 12}) and yttrium aluminum garnet doped with neodymium (Nd:YAG) single crystals were grown by the Czochralski technique. Themore » critical diameter and the critical rate of rotation were calculated. Suitable polishing and etching solutions were determined. As a result of our experiments, the transparent YAG and pale pink Nd:YAG single crystals were produced. The obtained crystals were studied by X-ray diffraction, Raman and IR spectroscopy. The crystal structure was confirmed by XRD. The 15 Raman and 17 IR modes were observed. The Raman and IR spectroscopy results are in accordance with X-ray diffraction analysis. The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. The absence of a core was confirmed by viewing polished crystal slices. Also, it is important to emphasize that the obtained Nd:YAG single crystal has a concentration of 0.8 wt.% Nd{sup 3+} that is characteristic for laser materials.« less

The Great Fallacy of the H Plus Ion and the True Nature of H30 Plus.

ERIC Educational Resources Information Center

Giguere, Paul A.

1979-01-01

Experimental and theoretical data are presented which verifies the existence of the hydronium ion. This existence was confirmed directly by x-ray and neutron diffraction in hydrochloric acid. Recommended is the abandonment of the erroneous hydrogen ion formulation and names such as proton hydrate. (BT)

The Confirmation of the Inverse Square Law Using Diffraction Gratings

ERIC Educational Resources Information Center

Papacosta, Pangratios; Linscheid, Nathan

2014-01-01

Understanding the inverse square law, how for example the intensity of light or sound varies with distance, presents conceptual and mathematical challenges. Students know intuitively that intensity decreases with distance. A light source appears dimmer and sound gets fainter as the distance from the source increases. The difficulty is in…

Antibacterial Carbon Nanotubes by Impregnation with Copper Nanostructures

NASA Astrophysics Data System (ADS)

Palza, Humberto; Saldias, Natalia; Arriagada, Paulo; Palma, Patricia; Sanchez, Jorge

2017-08-01

The addition of metal-based nanoparticles on carbon nanotubes (CNT) is a relevant method producing multifunctional materials. In this context, CNT were dispersed in an ethanol/water solution containing copper acetate for their impregnation with different copper nanostructures by either a non-thermal or a thermal post-synthesis treatment. Our simple method is based on pure CNT in an air atmosphere without any other reagents. Particles without thermal treatment were present as a well-dispersed layered copper hydroxide acetate nanostructures on CNT, as confirmed by scanning and transmission (TEM) electron microscopies, and showing a characteristic x-ray diffraction peak at 6.6°. On the other hand, by thermal post-synthesis treatment at 300°C, these layered nanostructures became Cu2O nanoparticles of around 20 nm supported on CNT, as confirmed by TEM images and x-ray diffraction peaks. These copper nanostructures present on the CNT surface rendered antibacterial behavior to the resulting hybrid materials against both Staphylococcus aureus and Escherichia coli. These findings present for the first time a simple method for producing antibacterial CNT by direct impregnation of copper nanostructures.

Effect of different annealing condition on the structural and magnetic properties of Mn2NiGa Heusler alloys

NASA Astrophysics Data System (ADS)

Vagadia, Megha; Hester, James; Nigam, A. K.

2018-04-01

We studied the effect of different annealing conditions on structural and magnetic properties of Mn2NiGa Heusler alloys. Reitveld refinement of neutron diffraction pattern at RT confirms the tetragonal structure with cubic phase for I-W quenched alloy whereas Le Bail fitting trials performed on neutron diffraction pattern collected for other three alloys confirm 7M monoclinic structure with cubic phase. It is found that starting and finish temperatures associated with martensite and austenite phase transformation depends strongly on the cooling rate corresponding to different cooling techniques. Slow furnace cooled sample possesses the highest martensite start temperature above room temperature ˜ 326K which decreases to ˜ 198K for ice -water quenched sample. Variation in the drop in the magnetization around MS obtained upon warming from martensite to austenite phase under ZFC cycle suggests that change in the cooling condition strongly affects the magnetization in the low temperature martensite phase. Present results suggest that by varying the cooling rate, martensite transformation as well as the martensite structure can be tuned.

Spectroscopic characterization of zinc oxide nanorods synthesized by solid-state reaction

NASA Astrophysics Data System (ADS)

Prasad, Virendra; D'Souza, Charlene; Yadav, Deepti; Shaikh, A. J.; Vigneshwaran, Nadanathangam

2006-09-01

Well-crystallized zinc oxide nanorods have been fabricated by single step solid-state reaction using zinc acetate and sodium hydroxide, at room temperature. The sodium lauryl sulfate (SLS) stabilized zinc oxide nanorods were characterized by using X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and photoluminescence spectroscopy. The X-ray diffraction revealed the wurtzite structure of zinc oxide. The size estimation by XRD and TEM confirmed that the ZnO nanorods are made of single crystals. The growth of zinc oxide crystals into rod shape was found to be closely related to its hexagonal nature. The mass ratio of SLS:ZnO in the nanorods was found to be 1:10 based on the thermogravimetric analysis. Blue shift of photoluminescence emission was noticed in the ZnO nanorods when compared to that of ZnO bulk. FT-IR analysis confirmed the binding of SLS with ZnO nanorods. Apart from ease of preparation, this method has the advantage of eco-friendliness since the solvent and other harmful chemicals were eliminated in the synthesis protocol.

X-ray diffraction, spectroscopic and mechanical studies on potential organic NLO materials of metaNitroaniline and N-3-Nitrophenyl Acetamide single crystals

NASA Astrophysics Data System (ADS)

Senthil, S.; Madhavan, J.

2015-02-01

In the present paper, attempts were made to grow good quality metaNitroaniline (mNA) and N-3-Nitrophenyl (3-NAA) single crystals. The lattice parameter values from the Powder X-ray diffraction pattern confirms that mNA belongs to orthorhombic crystal system with the unit cell parameter values of a = 6.501 Å, b = 19.330 Å and c = 5.082 Å with space group Pbc21. Similarly the powder XRD data indicates that 3-NAA crystal retained its monoclinic structure with lattice parameter values a = 9.762 Å, b =13.287 Å, c =13.226 Å, and β = 102.99°. Investigation has been carried out to assign the vibrational frequencies of the grown crystals by Fourier Transform infrared spectroscopy technique. The SHG efficiency of mNA and 3NAA was determined by Kurtz and Perry powder technique. The Optical absorption study confirms the suitability of the crystals for device applications. The mechanical properties of the grown crystals have been studied using Vickers microhardness tester.

Mechanical and physicochemical properties of AlN thin films obtained by pulsed laser deposition

NASA Astrophysics Data System (ADS)

Cibert, C.; Tétard, F.; Djemia, P.; Champeaux, C.; Catherinot, A.; Tétard, D.

2004-10-01

AlN thin films have been deposited on Si(100) substrates by a pulsed laser deposition method. The deposition parameters (pressure, temperature, purity of target) play an important role in the mechanical and physicochemical properties. The films have been characterized using X-ray diffraction, atomic force microscopy, Brillouin light scattering, Fourier transform infrared spectroscopy and wettability testing. With a high purity target of AlN and a temperature deposition of 750 ∘C, the measured Rayleigh wave velocity is close to the one previously determined for AlN films grown at high temperature by metal-organic chemical vapour deposition. Growth of nanocrystalline AlN at low temperature and of AlN film with good crystallinity for samples deposited at higher temperature is confirmed by infrared spectroscopy, as it was by atomic force microscopy, in agreement with X-ray diffraction results. A high hydrophobicity has been measured with zero polar contribution for the surface energy. These results confirm that films made by pulsed laser deposition of pure AlN at relatively low temperature have good prospects for microelectromechanical systems applications.

A novel structure of gel grown strontium cyanurate crystal and its structural, optical, electrical characterization

NASA Astrophysics Data System (ADS)

Divya, R.; Nair, Lekshmi P.; Bijini, B. R.; Nair, C. M. K.; Gopakumar, N.; Babu, K. Rajendra

2017-12-01

Strontium cyanurate crystals with novel structure and unique optical property like mechanoluminescence have been grown by conventional gel method. Transparent crystals were obtained. The single crystal X-ray diffraction analysis reveals the exquisite structure of the grown crystal. The crystal is centrosymmetric and has a three dimensional polymeric structure. The powder X ray diffraction analysis confirms its crystalline nature. The functional groups present in the crystal were identified by Fourier transform infrared spectroscopy. Elemental analysis confirmed the composition of the complex. A study of thermal properties was done by thermo gravimetric analysis and differential thermal analysis. The optical properties like band gap, refractive index and extinction coefficient were evaluated from the UV visible spectral analysis. The etching study was done to reveal the dislocations in the crystal which in turn explains mechanoluminescence emission. The mechanoluminescence property exhibited by the crystal makes it suitable for stress sensing applications. Besides being a centrosymmetric crystal, it also exhibits NLO behavior. Dielectric properties were studied and theoretical calculations of Fermi energy, valence electron plasma energy, penn gap and polarisability have been done.

Nano-Crystalline Thermally Evaporated Bi2Se3 Thin Films Synthesized from Mechanically Milled Powder

NASA Astrophysics Data System (ADS)

Amara, A.; Abdennouri, N.; Drici, A.; Abdelkader, D.; Bououdina, M.; Chaffar Akkari, F.; Khemiri, N.; Kanzari, M.; Bernède, J. C.

2017-08-01

Bi2Se3 powder has been successfully synthesized via mechanical ball milling of bismuth and selenium as starting materials. X-ray diffraction characterization revealed the formation of the rhombohedral and orthorhombic phases of Bi2Se3 material belonging to systems with space groups R\\bar{3}m and Pbnm, respectively. The advantageous last finding is confirmed by the Rietveld refinement of the x-ray diffraction data. Furthermore, the analysis of the x-ray data of thermally deposited thin films revealed that both orthorhombic and rhombohedral phases are coexisting in the layer. The morphology of the ball milled powder was studied by scanning electron microscopy. The phase formation of the material is confirmed by Raman spectroscopy. M-H (Magnetization versus Magnetic field) curve indicates that Bi2Se3 powder has a ferromagnetic behavior. Additionally, absorbance and transmittance measurements were carried out on the obtained thermally evaporated thin films and yielded a band gap of 1.33 eV supporting the potential application of the heterogeneous rhombohedral/orthorhombic Bi2Se3 material in photovoltaics.

Optical, Magnetic and Photocatalytic Activity Studies of Li, Mg and Sr Doped and Undoped Zinc Oxide Nanoparticles.

PubMed

Shanthi, S I; Poovaragan, S; Arularasu, M V; Nithya, S; Sundaram, R; Magdalane, C Maria; Kaviyarasu, K; Maaza, M

2018-08-01

Nanoparticles of Li, Mg and Sr doped and undoped zinc oxide was prepared by simple precipitation method. The structural, optical, and magnetic properties of the samples were investigated by the Powder X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Fourier Transform Infrared (FTIR) spectroscopy, Ultra-violet Visible spectroscopy (UV-vis) spectra, Photoluminescence (PL) and Vibrational Sample Magnetometer (VSM). The Powder X-ray diffraction data confirm the formation of hexagonal wurtzite structure of all doped and undoped ZnO. The SEM photograph reveals that the pores availability and particles size in the range of 10 nm-50 nm. FTIR and UV-Visible spectra results confirm the incorporation of the dopant into the ZnO lattice nanostructure. The UV-Visible spectra indicate that the shift of blue region (lower wavelength) due to bandgap widening. Photoluminescence intensity varies with doping due to the increase of oxygen vacancies in prepared ZnO. The pure ZnO exist paramagnetic while doped (Li, Mg and Sr) ZnO exist ferromagnetic property. The photocatalytic activity of the prepared sample also carried out in detail.

Influence of Ar-irradiation on structural and nanomechanical properties of pure zirconium measured by means of GIXRD and nanoindentation techniques

NASA Astrophysics Data System (ADS)

Kurpaska, L.; Gapinska, M.; Jasinski, J.; Lesniak, M.; Sitarz, M.; Nowakowska-Langier, K.; Jagielski, J.; Wozniak, K.

2016-12-01

An effect of Ar-irradiation on structural and nanomechanical properties of pure zirconium at room temperature was investigated. In order to simulate the radiation damage, the argon ions were implanted into the pure zirconium coupons with fluences ranging from 1 × 1015 to 1 × 1017 cm-2. Prior to irradiation, zirconium samples were chemically polished with a solution of HF/HNO3/H2O. Structural properties of the implanted layer were studied using Grazing Incidence X-Ray Diffraction (GIXRD) technique. The nanomechanical properties of the material were measured by means of nanoindentation technique. The obtained results revealed correlation between Ar-implantation fluence, hardness and structural properties (as confirmed by the modification of the diffraction peaks). Material hardening and peak shift & broadening in GIXD spectra were associated with the local increase of micro-strains, which is related to the increased density of type - dislocation loops. Presented study confirms that the structural changes induced by ion irradiation are directly linked to the mechanical response of the sample.

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

Syntheses, structures and properties of two new coordination polymers based on D-camphoric acid and 2-phenyl-4,6-diamino-1,3,5-triazine

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

Lun, Huijie; Yang, Jinghe; Jin, Linyu

2015-05-15

By hydrothermal method, two new coordination polymers [Co(ca)(phdat)]{sub n} (1), [Ni(ca)(phdat).0.125H{sub 2}O]{sub n} (2) (H{sub 2}ca=D-camphoric acid, phdat=2-phenyl-4,6-diamino-1,3,5-triazine) have been achieved and structurally characterized by IR, elemental analyses, X-ray single-crystal diffraction and TGA. The X-ray single-crystal diffraction reveals that compounds 1 and 2 are isostructural, both of which exhibit two-dimensional layered network built up from paddle-wheel Co{sub 2}(CO{sub 2}){sub 4}/Ni{sub 2}(CO{sub 2}){sub 4} SBUs by ca{sup 2−} ligand. In the existence of π…π stacking interactions between triazine rings and phenyl rings, the 3D networks are constructed with the hanging phdat filled between the neighboring layers. Furthermore, compounds 1–2 exhibit antiferromagneticmore » behavior and compound 2 displays a good activity for methanol oxidation. - Graphical abstract: Two new coordination compounds 1–2 have been synthesized and characterized by single-crystal X-ray diffractions, IR spectra, elemental analyses, thermogravimetric analyses, magnetic and electrochemical measurement. - Highlights: • This paper reports two new coordination polymers based on D-camphoric acid. • Both the compounds feather two-dimensional layered networks built up from paddle-wheel SBUs. • The magnetism and electrochemical property are investigated.« less

Effective increase in beam emittance by phase-space expansion using asymmetric Bragg diffraction.

PubMed

Chu, Chia-Hung; Tang, Mau-Tsu; Chang, Shih-Lin

2015-08-24

We propose an innovative method to extend the utilization of the phase space downstream of a synchrotron light source for X-ray transmission microscopy. Based on the dynamical theory of X-ray diffraction, asymmetrically cut perfect crystals are applied to reshape the position-angle-wavelength space of the light source, by which the usable phase space of the source can be magnified by over one hundred times, thereby "phase-space-matching" the source with the objective lens of the microscope. The method's validity is confirmed using SHADOW code simulations, and aberration through an optical lens such as a Fresnel zone plate is examined via matrix optics for nano-resolution X-ray images.

Cost-effective large-scale fabrication of diffractive optical elements by using conventional semiconducting processes.

PubMed

Yoo, Seunghwan; Song, Ho Young; Lee, Junghoon; Jang, Cheol-Yong; Jeong, Hakgeun

2012-11-20

In this article, we introduce a simple fabrication method for SiO(2)-based thin diffractive optical elements (DOEs) that uses the conventional processes widely used in the semiconductor industry. Photolithography and an inductively coupled plasma etching technique are easy and cost-effective methods for fabricating subnanometer-scale and thin DOEs with a refractive index of 1.45, based on SiO(2). After fabricating DOEs, we confirmed the shape of the output light emitted from the laser diode light source and applied to a light-emitting diode (LED) module. The results represent a new approach to mass-produce DOEs and realize a high-brightness LED module.

Native MS and ECD Characterization of a Fab-Antigen Complex May Facilitate Crystallization for X-ray Diffraction

NASA Astrophysics Data System (ADS)

Zhang, Ying; Cui, Weidong; Wecksler, Aaron T.; Zhang, Hao; Molina, Patricia; Deperalta, Galahad; Gross, Michael L.

2016-07-01

Native mass spectrometry (MS) and top-down electron-capture dissociation (ECD) combine as a powerful approach for characterizing large proteins and protein assemblies. Here, we report their use to study an antibody Fab (Fab-1)-VEGF complex in its near-native state. Native ESI with analysis by FTICR mass spectrometry confirms that VEGF is a dimer in solution and that its complex with Fab-1 has a binding stoichiometry of 2:2. Applying combinations of collisionally activated dissociation (CAD), ECD, and infrared multiphoton dissociation (IRMPD) allows identification of flexible regions of the complex, potentially serving as a guide for crystallization and X-ray diffraction analysis.

Non-destructive detection of cross-sectional strain and defect structure in an individual Ag five-fold twinned nanowire by 3D electron diffraction mapping.

PubMed

Fu, Xin; Yuan, Jun

2017-07-24

Coherent x-ray diffraction investigations on Ag five-fold twinned nanowires (FTNWs) have drawn controversial conclusions concerning whether the intrinsic 7.35° angular gap could be compensated homogeneously through phase transformation or inhomogeneously by forming disclination strain field. In those studies, the x-ray techniques only provided an ensemble average of the structural information from all the Ag nanowires. Here, using three-dimensional (3D) electron diffraction mapping approach, we non-destructively explore the cross-sectional strain and the related strain-relief defect structures of an individual Ag FTNW with diameter about 30 nm. The quantitative analysis of the fine structure of intensity distribution combining with kinematic electron diffraction simulation confirms that for such a Ag FTNW, the intrinsic 7.35° angular deficiency results in an inhomogeneous strain field within each single crystalline segment consistent with the disclination model of stress-relief. Moreover, the five crystalline segments are found to be strained differently. Modeling analysis in combination with system energy calculation further indicates that the elastic strain energy within some crystalline segments, could be partially relieved by the creation of stacking fault layers near the twin boundaries. Our study demonstrates that 3D electron diffraction mapping is a powerful tool for the cross-sectional strain analysis of complex 1D nanostructures.

Green synthesis of silver nanoparticles from aqueous leaf extract of Pomegranate (Punica granatum) and their anticancer activity on human cervical cancer cells

NASA Astrophysics Data System (ADS)

Sarkar, Sonia; Kotteeswaran, Venkatesan

2018-06-01

Plants contain different important phytochemicals that can be used as a potential treatment for various ailments including cancer. The green synthesis of silver nanoparticles from the extract of different plant parts has gained a wide range of engrossment among the researchers due to its unique optical and structural property. The aim of this study is green synthesis of silver nanoparticles from the aqueous leaf extract of pomegranate (Punica granatum) and to investigate its anticancer activity on human cervical cancer cells (HeLa). The synthesis of silver nanoparticle was depicted by the colour change from golden yellowish to dark brownish, UV-visible spectral analysis gave a characteristic surface plasmon absorption peak at . Further morphological characterization was done by Zeta potential where the size analysis was depicted to be 46.1 nm and zeta potential as . Fourier transform infrared spectroscopy (FTIR) inferred 3 intense sharp peaks at , , , confirmed the presence of flavonoids and polyphenols. The scanning electron microscopy (SEM) analysis with energy diffraction spectroscopy (EDS) confirmed the presence of silver nanoparticles with size ranged from to . X-ray diffraction (XRD) confirmed the crystallographic nature of silver. The cell proliferation activity of nanoparticles was tested by 3, ‑4, 5 dimethylthiazol-2,5 diphenyl tetrazolium bromide (MTT) assay where the inhibitory concentration () was found at inhibiting of HeLa cell line. The anticancer activity of nanoparticles was determined by lactate dehydrogenase (LDH) assay where showed of cytotoxicity. Furthermore, the anticancer property of nanoparticles was confirmed by the DNA fragmentation assay.

Geometry dependence of electron donating or accepting abilities of amine groups in 4,4‧-disulfanediylbis(methylene)dithiazol-2-amine: Pyramidal versus planar

NASA Astrophysics Data System (ADS)

Karabıyık, Hasan; Kırılmış, Cumhur; Karabıyık, Hande

2017-08-01

The molecular and crystal structure of the title compound in which two thiazole-2-amine rings are linked to each other by disulfide bridge (sbnd Csbnd Ssbnd Ssbnd Csbnd) were studied by single-crystal X-ray diffraction, FT-IR, NMR spectroscopy, quantum chemical calculations and topological analyses on the electron density. A novel synthesis route for the compounds having symmetrical disulfide bridge is reported. The most important result regarding the compound is about electron donating or accepting properties of the terminal amine groups. Planar amine group acts as an electron-donating group, while pyramidal amine behaves as electron-accepting group. This inference was confirmed by scrutiny of crystallographic geometry and quantum chemical studies. To ascertain underlying reasons for this fact, intermolecular interactions (Nsbnd H⋯N type H-bonds and Csbnd H···π interactions) were studied. These interactions involving aromatic thiazole rings are verified by topological electron density and Hirshfeld surface analyses. Intermolecular interactions do not have an effect on the differentiation in electron donating or accepting ability of amine groups, because both amine groups are involved in Nsbnd H⋯N type H-bonds. In methodological sense, it has been understood that Ehrenfest forces acting on electron density are useful theoretical probe to analyze intra-molecular charge transfer processes.

Elucidation of structure and nature of the PdO-Pd transformation using in situ PDF and XAS techniques.

PubMed

Keating, Jonathan; Sankar, Gopinathan; Hyde, Timothy I; Kohara, Shinji; Ohara, Koji

2013-06-14

The PdO-Pd phase transformation in a 4 wt% Pd/Al2O3 catalyst has been investigated using in situ X-ray absorption spectroscopy (XAS) and in situ X-ray total scattering (also known as high-energy X-ray diffraction) techniques. Both the partial and total pair distribution functions (PDF) from these respective techniques have been analysed in depth. New information from PDF analysis of total scattering data has been garnered using the differential PDF (d-PDF) approach where only correlations orginating from PdO and metallic Pd are extracted. This method circumvents problems encountered in characerising the catalytically active components due to the diffuse scattering from the disordered γ-Al2O3 support phase. Quantitative analysis of the palladium components within the catalyst allowed for the phase composition to be established at various temperatures. Above 850 °C it was found that PdO had converted to metallic Pd, however, the extent of reduction was of the order ca. 70% Pd metal and 30% PdO. Complementary in situ XANES and EXAFS were performed, with heating to high temperature and subsequent cooling in air, and the results of the analyses support the observations, that residual PdO is detected at elevated temperatures. Hysteresis in the transformation upon cooling is confirmed from XAS studies where reoxidation occurs below 680 °C.

Biocompatibility assessment of SiO2-TiO2 composite powder on MG63 osteoblast cell lines for orthopaedic applications.

PubMed

Chellappa, Maniickam; Thejaswini, Bezawada; Vijayalakshmi, Uthirapathy

2017-02-01

The objective of this study is to evaluate the biocompatibility of composite powder consisting of silica and titania (SiO 2 -TiO 2 ) for biomedical applications. The advancement of nanoscience and nanotechnology encourages researchers to actively participate in reinvention of existing materials with improved physical, chemical and biological properties. Hence, a composite/hybrid material has given birth of new materials with intriguing properties. In the present investigation, SiO 2 -TiO 2 composite powder was synthesised by sol-gel method and the prepared nanocomposite was characterised for its phase purity, functional groups, surface topography by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy. Furthermore, to understand the adverse effects of composite, biocompatibility test was analysed by cell culture method using MG63 osteoblast cell lines as a basic screening method. From the results, it was observed that typical Si-O-Ti peaks in FT-IR confirms the formation of composite and the crystallinity of the composite powder was analysed by XRD analysis. Further in vitro biocompatibility and acridine orange results have indicated better biocompatibility at different concentrations on osteoblast cell lines. On the basis of these observations, we envision that the prepared silica-titania nanocomposite is an intriguing biomaterial for better biomedical applications.

STRUCTURAL ANALYSIS OF THE COMBUSTION SYNTHESIZED Y3+ DOPED CERIA (Ce0.9Y0.1O1.95)

NASA Astrophysics Data System (ADS)

Jeyanthi, C. Esther; Siddheswaran, R.; Kumar, Pushpendra; Mangalaraja, R. V.; Siva Shankar, V.; Rajarajan, K.

2013-07-01

Y3+ doped CeO2 nanopowders (Ce0.9Y0.1O1.95, abbreviated as YDC) were synthesized by citrate-nitrate-auto combustion process using cerium nitrate hexahydrate, yttrium nitrate hexahydrate and citric acid. The as-synthesized powders were calcined at 700°C and converted into dense bodies followed by sintering at 1200°C. The microstructure of the synthesized powders and sintered bodies were examined by scanning electron microscopy (SEM). The surface morphology of the nanoparticles and clusters were also analysed by transmission electron microscopy (TEM). The particles size of the YDC was found to be in the range from 10 to 30 nm, which is in good agreement with the crystallite size calculated from X-ray peak broadening method. Also, the X-ray diffraction confirmed that the Ce0.9Y0.1O1.95 crystallizes as the cubic fluorite structure of pure ceria. The optical absorption by functional molecules, impurities and oxygen vacancies were analysed by FTIR and Raman spectroscopic studies. From the FTIR spectrum, the absorption peak found at 530 cm-1 is attributed to the vibrations of metal-oxygen bonds. The characteristic Raman peak was found to be 468 cm-1, and the minute absorption of oxygen vacancies were observed in the region 500-640 cm-1.

Physico-chemical analyses of Hispano-Moresque lustred ceramic: a precursor for Italian majolica?

NASA Astrophysics Data System (ADS)

Chabanne, D.; Bouquillon, A.; Aucouturier, M.; Dectot, X.; Padeletti, G.

2008-07-01

The paper presents a comprehensive physico-chemical investigation on a series of Hispano-Moresque objects produced in the eastern Spain workshops between the XIV and XVIII centuries and fragments from XII century, in order to compare them with the Italian Renaissance majolica production. The techniques used are mainly non-destructive (ion beam analyses and X-ray diffraction), sometimes complemented by SEM observation and microanalysis, and electrothermal atomic emission spectrometry. Such methods allow a full description of the terra cotta, of the glaze and of the different surface layers which constitute the lustre decoration indicating individual elemental composition and thickness of each layer containing or not metallic nanoparticles. Principal results show the following: i) a constant source of supply for the eastern Spain terra cotta; ii) a significant change in the composition of the Spanish glazes around the XVII century, with the disappearance of the opacifying tin oxide addition; iii) significant evolutions in the structure and composition of the lustre layers, in particular related to the presence or not of a metal-free surface glaze film and its thickness; iv) interesting analogies and differences with the Italian majolica; v) confirmation of the change in the quality of blue pigment during XVI century, already evidenced by the authors in previous publications. A discussion about the transmission of the lustre technique between eastern Spain and Italy at the Renaissance period is proposed.

A comprehensive overview on the structure and comparison of magnetic properties of nanocrystalline synthesized by a thermal treatment method

NASA Astrophysics Data System (ADS)

Naseri, Mahmoud Goodarz; Halimah, M. K.; Dehzangi, Arash; Kamalianfar, Ahmad; Saion, Elias B.; Majlis, Burhanuddin Y.

2014-03-01

This study reports the simple synthesis of MFe2O4 (where M=Zn, Mn and Co) nanostructures by a thermal treatment method, followed by calcination at various temperatures from 723 to 873 K. Poly(vinyl pyrrolidon) (PVP) was used as a capping agent to stabilize the particles and prevent them from agglomeration. The pyrolytic behaviors of the polymeric precursor were analyzed by use of simultaneous thermo-gravimetry analyses (TGA) and derivative thermo-gravimetry (DTG) analyses. The characterization studies were conducted by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Fourier transform infrared spectroscopy (FT-IR) confirmed the presence of metal oxide bands for all the calcined samples. Magnetic properties were demonstrated by a vibrating sample magnetometer (VSM), which displayed that the calcined samples exhibited different types of magnetic behavior. The present study also substantiated that magnetic properties of ferrite nanoparticles prepared by the thermal treatment method, from viewing microstructures of them, can be explained as the results of the two important factors: cation distribution and impurity phase of α-Fe2O3. These two factors are subcategory of the preparation method which is related to macrostructure of ferrite. Electron paramagnetic resonance (EPR) spectroscopy showed the existence of unpaired electrons ZnFe2O4 and MnFe2O4 nanoparticles while it did not exhibit resonance signal for CoFe2O4 nanoparticles.

New experimental diffractive-optical data on E.Land's Retinex mechanism in human color vision: Part II

NASA Astrophysics Data System (ADS)

Lauinger, N.

2007-09-01

A better understanding of the color constancy mechanism in human color vision [7] can be reached through analyses of photometric data of all illuminants and patches (Mondrians or other visible objects) involved in visual experiments. In Part I [3] and in [4, 5 and 6] the integration in the human eye of the geometrical-optical imaging hardware and the diffractive-optical hardware has been described and illustrated (Fig.1). This combined hardware represents the main topic of the NAMIROS research project (nano- and micro- 3D gratings for optical sensors) [8] promoted and coordinated by Corrsys 3D Sensors AG. The hardware relevant to (photopic) human color vision can be described as a diffractive or interference-optical correlator transforming incident light into diffractive-optical RGB data and relating local RGB onto global RGB data in the near-field behind the 'inverted' human retina. The relative differences at local/global RGB interference-optical contrasts are available to photoreceptors (cones and rods) only after this optical pre-processing.

Quantitative X-ray diffraction and fluorescence analysis of paint pigment systems : final report.

DOT National Transportation Integrated Search

1978-01-01

This study attempted to correlate measured X-ray intensities with concentrations of each member of paint pigment systems, thereby establishing calibration curves for the quantitative analyses of such systems.

Iridescence of a shell of mollusk Haliotis Glabra

NASA Astrophysics Data System (ADS)

Tan, T. L.; Wong, D.; Lee, Paul

2004-10-01

Pearls and shells of some mollusks are attractive inorganic materials primarily owing to the beauty of their natural lustrous and iridescent surface. The iridescent colors can be explained by diffraction or interference or both, depending on the microstructure of the surface. Strong iridescent colors are very evident on the polished shell of the mollusk Haliotis Glabra, commonly known as abalone. It would be interesting to study how these colors are produced on the surface of the shell. By using a scanning electron microscope (SEM), the surface of the shell is found to have a fine-scale diffraction grating structure, and stacks of thin crystalline nacreous layers or platelets are found below the surface. These observations suggest that the iridescent colors are caused by both diffraction and interference. From measurements done on the diffraction patterns that were obtained using a He-Ne laser illuminating the shell, the groove width of the grating structure was derived. Good agreement was found between the derived groove density by diffraction and that measured directly using the SEM. The crystalline structure of the nacreous layers of the shell is studied using Fourier transform infrared spectroscopy and SEM observations. The infrared absorption peaks of 700, 713, 862 and 1083 cm-1 confirmed that the nacre of the shell is basically aragonite. The strong iridescent colors of the shell are the result of high groove density on the surface which causes diffraction. The uniform stacking of layers of nacre below the surface of the shell also causes interference effects that contribute to the iridescent colors.

Transmission electron microscope studies of extraterrestrial materials

NASA Technical Reports Server (NTRS)

Keller, Lindsay P.

1995-01-01

Transmission Electron Microscopy, X-Ray spectrometry and electron-energy-loss spectroscopy are used to analyse carbon in interplanetary dust particles. Optical micrographs are shown depicting cross sections of the dust particles embedded in sulphur. Selected-area electron diffraction patterns are shown. Transmission Electron Microscope specimens of lunar soil were prepared using two methods: ion-milling and ultramicrotomy. A combination of high resolution TEM imaging and electron diffraction is used to characterize the opaque assemblages. The opaque assemblages analyzed in this study are dominated by ilmenite with lesser rutile and spinel exsolutions, and traces of Fe metal.

Rapid synthesis of flower shaped Cu{sub 2}ZnSnS{sub 4} nanoparticles by microwave irradiation for solar cell application

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

Ansari, Mohd Zubair, E-mail: mhd.zubair1@gmail.com; Khare, Neeraj

Single phase Cu{sub 2}ZnSnS{sub 4} (CZTS) nanoparticles have been synthesized by the microwave-assisted solution method in a one step process. Structural, morphological and optical characterizations of the CZTS nanoparticles have been carried out. X-ray diffraction confirms the single phase formation of CZTS nanoparticles with kesterite structure. SEM confirms the homogenous distribution of CZTS nanoparticles flower like assemblies. High resolution TEM image confirms the good crystallinity of the CZTS nanoparticles with the average grain size ~20 nm. The CZTS nanoparticles have strong optical absorption in the visible region with direct band gap as ~1.6 eV which is optimal for photovoltaic application.

Au Nanoparticle Sub-Monolayers Sandwiched between Sol-Gel Oxide Thin Films

PubMed Central

Della Gaspera, Enrico; Menin, Enrico; Sada, Cinzia

2018-01-01

Sub-monolayers of monodisperse Au colloids with different surface coverage have been embedded in between two different metal oxide thin films, combining sol-gel depositions and proper substrates functionalization processes. The synthetized films were TiO2, ZnO, and NiO. X-ray diffraction shows the crystallinity of all the oxides and verifies the nominal surface coverage of Au colloids. The surface plasmon resonance (SPR) of the metal nanoparticles is affected by both bottom and top oxides: in fact, the SPR peak of Au that is sandwiched between two different oxides is centered between the SPR frequencies of Au sub-monolayers covered with only one oxide, suggesting that Au colloids effectively lay in between the two oxide layers. The desired organization of Au nanoparticles and the morphological structure of the prepared multi-layered structures has been confirmed by Rutherford backscattering spectrometry (RBS), Secondary Ion Mass Spectrometry (SIMS), and Scanning Electron Microscopy (SEM) analyses that show a high quality sandwich structure. The multi-layered structures have been also tested as optical gas sensors. PMID:29538338

Microstructure, Texture and Mechanical Properties of Titanium Grade 2 Processed by ECAP (Route C)

NASA Astrophysics Data System (ADS)

Wroński, M.; Wierzbanowski, K.; Wojtas, D.; Szyfner, E.; Valiev, R. Z.; Kawałko, J.; Berent, K.; Sztwiertnia, K.

2018-03-01

In the present work the properties of titanium grade 2 after ECAP processing with original route and regimes (route C, channel angle Φ= 120°, deformation temperature 300 °C, number of passes up to 8) were examined. Texture development and microstructure parameters after ECAP processing and after recrystallization were determined using electron back scatter diffraction and analysed. A significant increase of the mechanical strength accompanied by some increase of ductility was observed in the deformed samples. The kernel average misorientation and average grain orientation spread were strongly increased after deformation, which confirms the material refinement and fragmentation. The proportion of low angle boundaries increased after four ECAP passes, but after four consecutive passes high angle grain boundaries became predominant. No deformation twins were observed after four and eight ECAP passes. The material recrystallized after deformation retained a fine grain microstructure. The textures of deformed and recrystallized samples were determined. It was found that texture after 8 passes is more homogeneous that that after 4 passes, which partly explains higher ductility of this first sample.

Monoclinic tridymite in clast-rich impact melt rock from the Chesapeake Bay impact structure

USGS Publications Warehouse

Jackson, John C.; Horton, J. Wright; Chou, I-Ming; Belkin, Harvey E.

2011-01-01

X-ray diffraction and Raman spectroscopy confirm a rare terrestrial occurrence of monoclinic tridymite in clast-rich impact melt rock from the Eyreville B drill core in the Chesapeake Bay impact structure. The monoclinic tridymite occurs with quartz paramorphs after tridymite and K-feldspar in a microcrystalline groundmass of devitrified glass and Fe-rich smectite. Electron-microprobe analyses revealed that the tridymite and quartz paramorphs after tridymite contain different amounts of chemical impurities. Inspection by SEM showed that the tridymite crystal surfaces are smooth, whereas the quartz paramorphs contain irregular tabular voids. These voids may represent microporosity formed by volume decrease in the presence of fluid during transformation from tridymite to quartz, or skeletal growth in the original tridymite. Cristobalite locally rims spherulites within the same drill core interval. The occurrences of tridymite and cristobalite appear to be restricted to the thickest clast-rich impact melt body in the core at 1402.02–1407.49 m depth. Their formation and preservation in an alkali-rich, high-silica melt rock suggest initially high temperatures followed by rapid cooling.

Water-assisted growth of graphene on carbon nanotubes by the chemical vapor deposition method.

PubMed

Feng, Jian-Min; Dai, Ye-Jing

2013-05-21

Combining carbon nanotubes (CNTs) with graphene has been proved to be a feasible method for improving the performance of graphene for some practical applications. This paper reports a water-assisted route to grow graphene on CNTs from ferrocene and thiophene dissolved in ethanol by the chemical vapor deposition method in an argon flow. A double injection technique was used to separately inject ethanol solution and water for the preparation of graphene/CNTs. First, CNTs were prepared from ethanol solution and water. The injection of ethanol solution was suspended and water alone was injected into the reactor to etch the CNTs. Thereafter, ethanol solution was injected along with water, which is the key factor in obtaining graphene/CNTs. Transmission electron microscopy, scanning electron microscopy, X-ray diffraction, and Raman scattering analyses confirmed that the products were the hybrid materials of graphene/CNTs. X-ray photo-electron spectroscopy analysis showed the presence of oxygen rich functional groups on the surface of the graphene/CNTs. Given the activity of the graphene/CNT surface, CdS quantum dots adhered onto it uniformly through simple mechanical mixing.

Application of Membrane Crystallization for Minerals’ Recovery from Produced Water

PubMed Central

Ali, Aamer; Quist-Jensen, Cejna Anna; Macedonio, Francesca; Drioli, Enrico

2015-01-01

Produced water represents the largest wastewater stream from oil and gas production. Generally, its high salinity level restricts the treatment options. Membrane crystallization (MCr) is an emerging membrane process with the capability to extract simultaneously fresh water and valuable components from various streams. In the current study, the potential of MCr for produced water treatment and salt recovery was demonstrated. The experiments were carried out in lab scale and semi-pilot scale. The effect of thermal and hydrodynamic conditions on process performance and crystal characteristics were explored. Energy dispersive X-ray (EDX) and X-ray diffraction (XRD) analyses confirmed that the recovered crystals are sodium chloride with very high purity (>99.9%), also indicated by the cubic structure observed by microscopy and SEM (scanning electron microscopy) analysis. It was demonstrated experimentally that at recovery factor of 37%, 16.4 kg NaCl per cubic meter of produced water can be recovered. Anti-scaling surface morphological features of membranes were also identified. In general, the study provides a new perspective of isolation of valuable constituents from produced water that, otherwise, is considered as a nuisance. PMID:26610581

Experimental study on cesium immobilization in struvite structures.

PubMed

Wagh, Arun S; Sayenko, S Y; Shkuropatenko, V A; Tarasov, R V; Dykiy, M P; Svitlychniy, Y O; Virych, V D; Ulybkina, Е А

2016-01-25

Ceramicrete, a chemically bonded phosphate ceramic, was developed for nuclear waste immobilization and nuclear radiation shielding. Ceramicrete products are fabricated by an acid-base reaction between magnesium oxide and mono potassium phosphate that has a struvite-K mineral structure. In this study, we demonstrate that this crystalline structure is ideal for incorporating radioactive Cs into a Ceramicrete matrix. This is accomplished by partially replacing K by Cs in the struvite-K structure, thus forming struvite-(K, Cs) mineral. X-ray diffraction and thermo-gravimetric analyses are used to confirm such a replacement. The resulting product is non-leachable and stable at high temperatures, and hence it is an ideal matrix for immobilizing Cs found in high-activity nuclear waste streams. The product can also be used for immobilizing secondary waste streams generated during glass vitrification of spent fuel, or the method described in this article can be used as a pretreatment method during glass vitrification of high level radioactive waste streams. Furthermore, it suggests a method of producing safe commercial radioactive Cs sources. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis, characterization and anticancer activity of new Schiff bases bearing neocryptolepine

NASA Astrophysics Data System (ADS)

Emam, Sanaa M.; El Sayed, Ibrahim E. T.; Ayad, Mohamed I.; Hathout, Heba M. R.

2017-10-01

The synthesis of new Shiff base ligands denoted L1, HL2 and HL3 starting from the appropriate aminoneocryptolepine and salicaldehyde were described. The chelation abilities of L1, HL2 and HL3 ligands towards Co(II), Ni(II), Cu(II) and Pd(II) salts have been studied. A series of square planar complexes containing Cu(II) salts, PdCl2 and octahedral chelates containing NiCl2, CoCl2 salts (2 and 7) have been isolated. Also, the pentacoordinated Co(II) complex [Co(L1)2Cl]·Cl.0.5H2O·1.25EtOH (1) has been prepared. The mode of bonding and geometrical structure of complexes has been confirmed by elemental analyses and different spectroscopic methods together with thermal, magnetic moment studies, molecular modeling and X-ray diffraction. Furthermore, the synthesized ligands, in comparison to some of their metal complexes were screened for their anticancer activity against colorectal adenocarcinoma (HT-29) cells. The results showed that Co(II) complexes (1 and 7) exhibited higher anticancer activity when compared to the corresponding ligands.

Fabrication of free-standing copper foils covered with highly-ordered copper nanowire arrays

NASA Astrophysics Data System (ADS)

Zaraska, Leszek; Sulka, Grzegorz D.; Jaskuła, Marian

2012-07-01

The through-hole nanoporous anodic aluminum oxide (AAO) membranes with relatively large surface area (ca. 2 cm2) were employed for fabrication of free-standing and mechanically stable copper foils covered with close-packed and highly-ordered copper nanowire arrays. The home-made AAO membranes with different pore diameters and interpore distances were fabricated via a two-step self-organized anodization of aluminum performed in sulfuric acid, oxalic acid and phosphoric acid followed by the pore opening/widening procedure. The direct current (DC) electrodeposition of copper was performed efficiently on both sides of AAO templates. The bottom side of the AAO templates was not insulated and consequently Cu nanowire arrays on thick Cu layers were obtained. The proposed template-assisted fabrication of free-standing copper nanowire array electrodes is a promising method for synthesis of nanostructured current collectors. The composition of Cu nanowires was confirmed by energy dispersive X-Ray spectroscopy (EDS) and X-ray diffraction (XRD) analyses. The structural features of nanowires were evaluated from field emission scanning electron microscopy (FE-SEM) images and compared with the characteristic parameters of anodic alumina membranes.

Some Structural Properties of the Mixed Lead-Magnesium Hydroxyapatites

NASA Astrophysics Data System (ADS)

Kaaroud, K.; Ben Moussa, S.; Brigui, N.; Badraoui, B.

2018-02-01

Lead-magnesium hydroxyapatite solid solutions Pb(10- x)Mg x (PO4)6(OH)2 have been prepared via a hydrothermal process. They were characterized by X-ray powder diffraction, Transmission Electron Microscopy (TEM), chemical and IR spectroscopic analyses. The results of the structural refinement indicated that the limits of lead-magnesium solid solutions ( x ≤ 1.5), a regular decrease of the lattice constant a and a preferential magnesium distribution in site S(I). Through the progressive replacement of Pb2+ ( r = 0.133 nm) by the smaller cation Mg2+ ( r = 0.072 nm), all interatomic distances decrease in accordance with the decrease of the cell parameters. According to what could be expected from the coordinance of the metallic sites S(I) (hexacoordination) and S(II) (heptacoordination), the small magnesium cation preferentially occupies the four sites S(I). The results of the TEM analysis confirm the presence of magnesium in the starting solution and reveals the decrease in the average size of crystals. The IR spectra show the presence of the absorption bands characteristic for the apatite structure.

Noble-gas-rich separates from the Allende meteorite

NASA Technical Reports Server (NTRS)

Ott, U.; Mack, R.; Chang, S.

1981-01-01

Predominantly carbonaceous HF/HCl-resistant residues from the Allende meteorite are studied. Samples are characterized by SEM/EDXA, X-ray diffraction, INAA, C, S, H, N, and noble gas analyses. Isotopic data for carbon show variations no greater than 5%, while isotopic data from noble gases confirm previously established systematics. Noble gas abundances correlate with those of C and N, and concomitant partial loss of C and normal trapped gas occur during treatments with oxidizing acids. HF/HCl demineralization of bulk meteorite results in similar fractional losses of C and trapped noble gases, which leads to the conclusion that various macromolecular carbonaceous substances serve as the main host phase for normal trapped noble gases and anomalous gases in acid-resistant residues, and as the carrier of the major part of trapped noble gases lost during HF/HCl demineralization. Limits on the possible abundances of dense mineralic host phases in the residues are obtained, and considerations of the nucleogenetic origin for CCF-XE indicate that carbonaceous host phases and various forms of organic matter in carbonaceous meteorites may have a presolar origin.

Nano-sized, quaternary titanium(IV) metal-organic frameworks with multidentate ligands.

PubMed

Baranwal, Balram Prasad; Singh, Alok Kumar

2010-12-01

Some mononuclear nano-sized, quaternary titanium(IV) complexes having the general formula [Ti(acac)(OOCR)2(SB)] (where Hacac=acetylacetone, R=C15H31 or C17H35, HSB=Schiff bases) have been synthesized using different multidentate ligands. These were characterized by elemental analyses, molecular weight determinations and spectral (FTIR, 1H NMR and powder XRD) studies. Conductance measurement indicated their non-conducting nature which may behave like insulators. Structural parameters like the values of limiting indices h, k, l, cell constants a, b, c, angles α, β, γ and particle size are calculated from powder XRD data for complex 1 which indicated nano-sized triclinic system in them. Bidentate chelating nature of acetylacetone, carboxylate and Schiff base anions in the complexes was established by their infrared spectra. Molecular weight determinations confirmed mononuclear nature of the complexes. On the basis of physico-chemical studies, coordination number 8 was assigned for titanium(IV) in the complexes. Transmission electron microscopy (TEM) and the selected area electron diffraction (SAED) studies indicated spherical particles with poor crystallinity. Copyright © 2010 Elsevier B.V. All rights reserved.

Structural comparative studies on new Mn(II), Cr(III) and Ru(III) complexes derived from 2,4,6-tri-(2-pyridyl)-1,3,5-triazine (TPTZ).

PubMed

Al-Assy, Waleed H; El-Askalany, Abdel Moneum H; Mostafa, Mohsen M

2013-12-01

The structure of a new Mn(II) complex, [Mn(TPTZ)Cl2(H2O)]⋅H2O, was established by a single crystal X-ray diffraction. Crystal data are as follow: monoclinic, P21/c,a = 8.7202 (3)Å, b = 11.5712 (4)Å, c = 20.8675 (9)Å, β=11 (18) × 1010, V = 2029.27 (13)Å(3), Z = 4. The HOMO, LUMO and other DFT parameters on the atoms have been calculated to confirm the geometry of the ligand and its complexes using material studio program. The complexes were characterized by elemental analyses, spectral, magnetic, thermal and cyclic voltammetry measurements. Electronic spectra and magnetic moments of the complexes suggest distorted-octahedral structures around the metal ions (Mn(II), Cr(III) and Ru(III)). The redox properties were investigated by cyclic voltammetry. Kinetic parameters were determined using Coats-Redfern and Horowitz-Metzger methods. The results of DNA studies of the metal complexes promised to be effective in tumour treatment. Copyright © 2013 Elsevier B.V. All rights reserved.

Synthesis of polycarbonate-r-polyethylene glycol copolymer for templated synthesis of mesoporous TiO2 films.

PubMed

Patel, Rajkumar; Kim, Jinkyu; Lee, Chang Soo; Kim, Jong Hak

2014-12-01

We synthesized a novel polycarbonate Z-r-polyethylene glycol (PCZ-r-PEG) copolymer by solution polycondensation. Successful synthesis of PCZ-r-PEG copolymer was confirmed by Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (1H-NMR), gel permeation chromatography (GPC), and transmission electron microscopy (TEM). PCZ-r-PEG copolymer was used as a structure-directing agent for fabrication of mesoporous thin film containing a titanium dioxide (TiO2) layer. To control the porosity of the resultant inorganic layer, the ratio of titanium(IV) isopropoxide (TTIP) to PCZ-r-PEG copolymer was varied. The structure and porosity of the resulting mesoporous films were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses. Mesoporous TiO2 films fabricated on an F-doped tin oxide (FTO) surface were used as photoanodes for quasi-solid-state dye-sensitized solar cells (qssDSSCs). The highest efficiency achieved was 3.3% at 100 mW/cm2 for a film thickness of 750 nm, which is high considering the thickness of TiO2 film, indicating the importance of the structure-directing agent.

Fabrication and characterization of aluminium hybrid composites reinforced with fly ash and silicon carbide through powder metallurgy

NASA Astrophysics Data System (ADS)

Bilal Naim Shaikh, Mohd; Arif, Sajjad; Arif Siddiqui, M.

2018-04-01

This paper reports the fabrication and characterization of aluminium hybrid composites (AMCs) reinforced with commonly available and inexpensive fly ash (FA, 0, 5, 10 and 15 wt.%) particles along silicon carbide (SiC) using powder metallurgy process. Scanning electron microscopy (SEM) and x-ray diffraction (XRD) were employed for microstructural characterization and phase identification respectively. Wear behaviour were investigated using pin-on-disc wear tester for the different combinations of wear parameters like load (10, 20 and 30 N), sliding speed (1.5, 2 and 2.5 m s‑1) and sliding distance (300, 600 and 900 m). SEM confirms the uniform distribution of FA and SiC in aluminium matrix. The hardness of Al/SiC/FA is increased by 20%–25% while wear rate decreased by 15%–40%. From wear analysis, sliding distance was the least significant parameter influencing the wear loss followed by applied load and sliding speed. To identify the mechanism of wear, worn out surface were also analysed by SEM.

Studies of Nano-structured Se77Sb23- x Ge x Thin Films Prepared by Physical Vapor Condensation Technique

NASA Astrophysics Data System (ADS)

Alvi, M. A.

2017-02-01

Bulk Se77Sb23- x Ge x material with x = 4 and 12 was prepared by employing a melt quench technique. Its amorphous as well as glassy nature was confirmed by x-ray diffraction analysis and nonisothermal differential scanning calorimetry measurements. The physical vapor condensation technique was applied to prepare nanostructured thin films of Se77Sb23- x Ge x material. The surface morphology of the films was examined using field-emission scanning electron microscopy, revealing average particle size between 20 nm and 50 nm. Systematic investigation of optical absorption data indicated that the optical transition was indirect in nature. The dark conductivity (dc conductivity) of nano-structured Se77Sb23- x Ge x thin films was also investigated at temperatures from 313 K to 463 K, revealing that it tended to increase with increasing temperature. Analyses of our experimental data also indicate that the conduction is due to thermally supported tunneling of charge carriers in confined states close to the band edges. The calculated values of activation energy agree well with the optical bandgap.

Bioactivity and structural properties of nanostructured bulk composites containing Nb2O5 and natural hydroxyapatite

NASA Astrophysics Data System (ADS)

Bonadio, T. G. M.; Sato, F.; Medina, A. N.; Weinand, W. R.; Baesso, M. L.; Lima, W. M.

2013-06-01

In this work, we investigate the bioactivity and structural properties of nanostructured bulk composites that are composed of Nb2O5 and natural hydroxyapatite (HAp) and are produced by mechanical alloying and powder metallurgy. X-ray diffraction and Raman spectroscopy data showed that the milling process followed by a heat treatment at 1000 °C induced chemical reactions along with the formation of the CaNb2O6, PNb9O25 and Ca3(PO4)2 phases. Rietveld refinement indicated significant changes in each phase weight fraction as a function of HAp concentration. These changes influenced the in vitro bioactivity of the material. XRD and FTIR analyses indicated that the composites exhibited bioactivity characteristics by forming a carbonated apatite layer when the composites were immersed in a simulated body fluid. The formed layers had a maximum thickness of 13 μm, as measured by confocal Raman spectroscopy and as confirmed by scanning electron microscopy. The results of this work suggest that the tested bulk composites are promising biomaterials for use in implants.

Fabrication of band gap engineered nanostructured tri-metallic (Mn-Co-Ti) oxide thin films

NASA Astrophysics Data System (ADS)

Mansoor, Muhammad Adil; Yusof, Farazila Binti; Nay-Ming, Huang

2018-04-01

In continuation of our previous studies on photoelectrochemical (PEC) properties of titanium based composite oxide thin films, an effort is made to develop thin films of 1:1:2 manganese-cobalt-titanium oxide composite, Mn2O3-Co2O3-4TiO2 (MCT), using Co(OAc)2 and a bimetallic manganese-titanium complex, [Mn2Ti4(TFA)8(THF)6(OH)4(O)2].0.4THF (1), where OAc = acetato, TFA = trifluoroacetato and THF = tetrahydrofuran, via aerosol-assisted chemical vapour deposition (AACVD) technique. The X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and energy dispersive X-ray (EDX) spectroscopic analyses confirmed formation of thin film of Mn2O3-Co2O3-4TiO2 composite material with uniformly distributed agglomerated particles. The average size of 39.5 nm, of the particles embedded inside agglomerates, was estimated by Scherer's equation. Further, UV-Vis spectroscopy was used to estimate the band gap of 2.62 eV for MCT composite thin film.

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.

Preparation and Properties of High-T(sub c) Bi-Pb-Sr-Ca-Cu-O Thick Film Superconductors on YSZ Substrates

NASA Technical Reports Server (NTRS)

Hooker, Matthew W.

1996-01-01

An evaluation of four firing profiles was performed to determine the optimum processing conditions for producing high-T(sub c) Bi-Pb-Sr-Ca-Cu-O thick films on yttria-stabilized zirconia substrates. Using these four profiles, the effects of sintering temperatures of 830-850 C and soak times of 0.5 to 12 hours were examined. In this study, T-c, zero values of 100 K were obtained using a firing profile in which the films were sintered for 1.5 to 2 hours at 840 to 845 C and then quenched to room temperature. X-ray diffraction analyses of these specimens confirmed the presence of the high-T(sub c) phase. Films which were similarly fired and furnace cooled from the peak processing temperature exhibited a two-step superconductive transition to zero resistance, with T-c,zero values ranging from 85 to 92 K. The other firing profiles evaluated in this investigation yielded specimens which either exhibited critical transition temperatures below 90 K or did not exhibit a superconductive transition above 77 K.

Structural comparative studies on new MnII, CrIII and RuIII complexes derived from 2,4,6-tri-(2-pyridyl)-1,3,5-triazine (TPTZ)

NASA Astrophysics Data System (ADS)

Al-Assy, Waleed H.; El-Askalany, Abdel Moneum H.; Mostafa, Mohsen M.

2013-12-01

The structure of a new MnII complex, [Mn(TPTZ)Cl2(H2O)]ṡH2O, was established by a single crystal X-ray diffraction. Crystal data are as follow: monoclinic, P21/c, a = 8.7202 (3) Å, b = 11.5712 (4) Å, c = 20.8675 (9) Å, β = 11 (18) × 1010, V = 2029.27 (13) Å3, Z = 4. The HOMO, LUMO and other DFT parameters on the atoms have been calculated to confirm the geometry of the ligand and its complexes using material studio program. The complexes were characterized by elemental analyses, spectral, magnetic, thermal and cyclic voltammetry measurements. Electronic spectra and magnetic moments of the complexes suggest distorted-octahedral structures around the metal ions (MnII, CrIII and RuIII). The redox properties were investigated by cyclic voltammetry. Kinetic parameters were determined using Coats-Redfern and Horowitz-Metzger methods. The results of DNA studies of the metal complexes promised to be effective in tumour treatment.

Structure, microstructure and infrared studies of Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3}-NaNbO{sub 3} ceramics

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

Roy, Sumit K., E-mail: sumit.sxc13@gmail.com; Singh, S. N., E-mail: snsphyru@gmail.com; Prasad, K., E-mail: k.prasad65@gmail.com

2016-05-06

Lead-free solid solutions (1-x)Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3}-xNaNbO{sub 3} (0 ≤ x ≤ 1.0) were prepared by conventional ceramic fabrication technique. X-ray diffraction and Rietveld refinement analyses of these ceramics were carried out using X’Pert HighScore Plus software to determine the crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that NaNbO{sub 3} with orthorhombic structure was completely diffused into Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3} lattice having the rhombohedral-tetragonal symmetry. EDS and SEM studies were carried out in order to evaluate the quality and purity of the compounds. SEM images showed a change in grain shapemore » with the increase of NaNbO{sub 3} content. FTIR spectra confirmed the formation of solid solution.« less

Parametric Rietveld refinement and magnetic characterization of superparamagnetic iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Pereira, Guilherme Ferreira Lemos; Costa, Fanny Nascimento; Souza, José Antonio; Haddad, Paula Silvia; Ferreira, Fabio Furlan

2018-06-01

This article describes the synthesis of two superparamagnetic iron oxide nanoparticles (SPIONs) covered with different ligands - hydrophobic (oleic acid (OA)) and hydrophilic (tetraethyl ammonium (TEA)) - and the investigation of the effects of thermal treatments on the crystal structure of TEA-SPIONs or OA-SPIONs using X-ray powder diffraction data and parametric Rietveld refinements; we stablished non-crystallographic models to describe how the oxidation processes take place with increasing temperatures for the different systems. The morphological and magnetic properties revealed the nanoparticles have a mean diameter of ∼10 nm in the solid state and are superparamagnetic at room temperature. Magnetization measurements confirmed the superparamagnetic state for both systems and revealed smaller particle sizes and narrower size distribution for OA-SPIONs than for TEA-SPIONs. The thermomagnetic analyses show only the ferrimagnetic phase transition of magnetite for OA-SPIONs while in the TEA-SPIONs, besides the ferrimagnetic phase transition there is the appearance of an antiferromagnetic one disclosing the evolution of hematite phase probably on the surface of magnetite due to thermal cycles.

Origin of anomalies and phase competitions around magnetic transition temperature in Pr0.7Ca0.3MnO3

NASA Astrophysics Data System (ADS)

Shah, Matiullah; Nadeem, M.; Atif, M.

2013-03-01

A polycrystalline sample of Pr0.7Ca0.3MnO3 is synthesized by the conventional solid-state reaction method and the phase formation is confirmed by x-ray diffraction. In this work, we addressed the phase competition issues in the vicinity of magnetic transition temperature and also established its correlation with oxygen contents of domains, disorder effects and heterogeneity in the material. The appearance and disappearance of anomaly in the vicinity of TC (128 K) with magnetic field is discussed in terms of establishment of short- and long-range networks between Mn3+ and Mn4+. Switching behaviour of two competing phases is analysed qualitatively and quantitatively, using an equivalent circuit model and magnetization analysis. The issue of coexisting phases is further substantiated using a simple depression angle approach of impedance plane plots. variable range hopping is found to be a better model than polaronic for explaining the transport properties of both competing phases below the magnetic transition temperature, 128 K.

High quality Y-type hexaferrite thick films for microwave applications by an economical and environmentally benign crystal growth technique

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

Hu, Bolin; Chen, Yajie, E-mail: y.chen@neu.edu; Gillette, Scott

2014-02-17

Thick barium hexaferrite Ba{sub 2}Zn{sub 2}Fe{sub 12}O{sub 22} (i.e., Zn{sub 2}Y) films having thicknesses of ∼100 μm were epitaxially grown on MgO (111) substrates using an environmentally benign ferrite-salt mixture by vaporizing the salt. X-ray diffraction pole figure analyses showed (00l) crystallographic alignment with little in plane dispersion confirming epitaxial growth. Saturation magnetization, 4πM{sub s}, was measured for as-grown films to be 2.51 ± 0.1 kG with an out of plane magnetic anisotropy field H{sub A} of 8.9 ± 0.1 kOe. Ferromagnetic resonance linewidth, as the peak-to-peak power absorption derivative at 9.6 GHz, was measured to be 62 Oe. These properties demonstrate a rapid, convenient, cost-effective, and nontoxic methodmore » of growing high quality thick crystalline ferrite films which could be used widely for microwave device applications.« less

Lead chromate detected as a source of atmospheric Pb and Cr (VI) pollution.

PubMed

Lee, Pyeong-Koo; Yu, Soonyoung; Chang, Hye Jung; Cho, Hye Young; Kang, Min-Ju; Chae, Byung-Gon

2016-10-25

Spherical black carbon aggregates were frequently observed in dust dry deposition in Daejeon, Korea. They were tens of micrometers in diameter and presented a mixture of black carbon and several mineral phases. Transmission electron microscopy (TEM) observations with energy-dispersive X-ray spectroscopy (EDS) and selected area diffraction pattern (SADP) analyses confirmed that the aggregates were compact and included significant amounts of lead chromate (PbCrO 4 ). The compositions and morphologies of the nanosized lead chromate particles suggest that they probably originated from traffic paint used in roads and were combined as discrete minerals with black carbon. Based on Pb isotope analysis and air-mass backward trajectories, the dust in Daejeon received a considerable input of anthropogenic pollutants from heavily industrialized Chinese cities, which implies that long-range transported aerosols containing PbCrO 4 were a possible source of the lead and hexavalent chromium levels in East Asia. Lead chromate should be considered to be a source of global atmospheric Pb and Cr(VI) pollution, especially given its toxicity.

Multielemental analyses of isomorphous Indian garnet gemstones by XRD and external pixe techniques.

PubMed

Venkateswarulu, P; Srinivasa Rao, K; Kasipathi, C; Ramakrishna, Y

2012-12-01

Garnet gemstones were collected from parts of Eastern Ghats geological formations of Andhra Pradesh, India and their gemological studies were carried out. Their study of chemistry is not possible as they represent mixtures of isomorphism nature, and none of the individual specimens indicate independent chemistry. Hence, non-destructive instrumental methodology of external PIXE technique was employed to understand their chemistry and identity. A 3 MeV proton beam was employed to excite the samples. In the present study geochemical characteristics of garnet gemstones were studied by proton induced X-ray emission. Almandine variety of garnet is found to be abundant in the present study by means of their chemical contents. The crystal structure and the lattice parameters were estimated using X-Ray Diffraction studies. The trace and minor elements are estimated using PIXE technique and major compositional elements are confirmed by XRD studies. The technique is found very useful in characterizing the garnet gemstones. The present work, thus establishes usefulness and versatility of the PIXE technique with external beam for research in Geo-scientific methodology. Copyright © 2012 Elsevier Ltd. All rights reserved.

Lead chromate detected as a source of atmospheric Pb and Cr (VI) pollution

NASA Astrophysics Data System (ADS)

Lee, Pyeong-Koo; Yu, Soonyoung; Chang, Hye Jung; Cho, Hye Young; Kang, Min-Ju; Chae, Byung-Gon

2016-10-01

Spherical black carbon aggregates were frequently observed in dust dry deposition in Daejeon, Korea. They were tens of micrometers in diameter and presented a mixture of black carbon and several mineral phases. Transmission electron microscopy (TEM) observations with energy-dispersive X-ray spectroscopy (EDS) and selected area diffraction pattern (SADP) analyses confirmed that the aggregates were compact and included significant amounts of lead chromate (PbCrO4). The compositions and morphologies of the nanosized lead chromate particles suggest that they probably originated from traffic paint used in roads and were combined as discrete minerals with black carbon. Based on Pb isotope analysis and air-mass backward trajectories, the dust in Daejeon received a considerable input of anthropogenic pollutants from heavily industrialized Chinese cities, which implies that long-range transported aerosols containing PbCrO4 were a possible source of the lead and hexavalent chromium levels in East Asia. Lead chromate should be considered to be a source of global atmospheric Pb and Cr(VI) pollution, especially given its toxicity.

Lead chromate detected as a source of atmospheric Pb and Cr (VI) pollution

PubMed Central

Lee, Pyeong-Koo; Yu, Soonyoung; Chang, Hye Jung; Cho, Hye Young; Kang, Min-Ju; Chae, Byung-Gon

2016-01-01

Spherical black carbon aggregates were frequently observed in dust dry deposition in Daejeon, Korea. They were tens of micrometers in diameter and presented a mixture of black carbon and several mineral phases. Transmission electron microscopy (TEM) observations with energy-dispersive X-ray spectroscopy (EDS) and selected area diffraction pattern (SADP) analyses confirmed that the aggregates were compact and included significant amounts of lead chromate (PbCrO4). The compositions and morphologies of the nanosized lead chromate particles suggest that they probably originated from traffic paint used in roads and were combined as discrete minerals with black carbon. Based on Pb isotope analysis and air-mass backward trajectories, the dust in Daejeon received a considerable input of anthropogenic pollutants from heavily industrialized Chinese cities, which implies that long-range transported aerosols containing PbCrO4 were a possible source of the lead and hexavalent chromium levels in East Asia. Lead chromate should be considered to be a source of global atmospheric Pb and Cr(VI) pollution, especially given its toxicity. PMID:27779222

Thermal analyses, spectral characterization and structural interpretation of Nd3+/Er3+ ions co-doped TeO2-ZnCl2 glasses system

NASA Astrophysics Data System (ADS)

Ahmed, Kasim F.; Ibrahim, Saeed O.; Sahar, Md. R.; Mawlud, Saman Q.; Khizir, Hersh A.

2017-09-01

The Nd3+/Er3+ ions co-doped in the system of zinc-tellurite with the composition of (70-2x)TeO2-30ZnCl2-xNd2O3-xEr2O3 concentration from 1.0 to 3.0 mol% (x=1, 2 and 3) glasses were prepared by using conventional melt-quenching technique. The amorphous nature of the glass been confirmed by using X-RAY Diffraction Spectroscopy. Thermal characteristic were determined using a DTA. The obtained results discussed in terms of the glass structure. The glass structure studied by means of FTIR. Seven significant vibrational peaks around 471, 687, 742, 768, 1632, 2833 and 3378 cm-1 which correspond to the structural bonding of the glass are observed in a range of 400-4000cm-1. The peaks observed are consistent with the stretching and bending vibrations of the Te-O, TeO4 trigonal bipyramids, TeO3 trigonal pyramids, Te-O-Te and OH linkages respectively.

Acid Green 1 removal from wastewater by layered double hydroxides

NASA Astrophysics Data System (ADS)

Elkhattabi, El Hassan; Lakraimi, Mohamed; Berraho, Moha; Legrouri, Ahmed; Hammal, Radouan; El Gaini, Layla

2018-03-01

The paper presents the removal of Acid Green 1 (AG1) from aqueous solutions by [Zn-Al-Cl]-layered double hydroxides (LDHs). The LDH was prepared by coprecipitation at constant pH. The affinity of this material for AG1 was studied as a function of contact time, pH of the solution, LDH dose and AG1/LDH mass ratio. It was found that 32 h are enough to reach the equilibrium with a maximum retention at pH 8 for an LDH dose of 100 mg and with an AG1/LDH mass ratio higher than 2. The adsorption isotherm is of L-type, as described by the Langmuir model. The results demonstrate that AG1 retention on LDHs occurs by adsorption on external surface when AG1/LDH mass ratio is equal or lower than 2 and by both adsorption and interlayer ion exchange for ratios higher than 2. A mechanism for the AG1 removal has been confirmed by X-ray diffraction, Fourier transform infrared spectroscopy, thermogravimetric-differential thermal analyses and scanning electron microscopy.

Synthesis and magnetic characterization of nickel ferrite nanoparticles prepared by co-precipitation route

NASA Astrophysics Data System (ADS)

Maaz, K.; Karim, S.; Mumtaz, A.; Hasanain, S. K.; Liu, J.; Duan, J. L.

2009-06-01

Magnetic nanoparticles of nickel ferrite (NiFe 2O 4) have been synthesized by co-precipitation route using stable ferric and nickel salts with sodium hydroxide as the precipitating agent and oleic acid as the surfactant. X-ray diffraction (XRD) and transmission electron microscope (TEM) analyses confirmed the formation of single-phase nickel ferrite nanoparticles in the range 8-28 nm depending upon the annealing temperature of the samples during the synthesis. The size of the particles ( d) was observed to be increasing linearly with annealing temperature of the sample while the coercivity with particle size goes through a maximum, peaking at ˜11 nm and then decreases for larger particles. Typical blocking effects were observed below ˜225 K for all the prepared samples. The superparamagnetic blocking temperature ( T B) was found to be increasing with increasing particle size that has been attributed to the increased effective anisotropy energy of the nanoparticles. The saturation moment of all the samples was found much below the bulk value of nickel ferrite that has been attributed to the disordered surface spins or dead/inert layer in these nanoparticles.

Theoretical and experimental morphologies of 4-aminobenzophenone (ABP) crystals

NASA Astrophysics Data System (ADS)

Wang, Qingwu; Sheen, D. B.; Shepherd, E. E. A.; Sherwood, J. N.; Simpson, G. S.; Hammond, R. B.

1997-11-01

The lattice energy (Elatt), slice energies (Eslice) and attachment energies (Eatt) of the different habit faces of ABP crystals have been calculated using the computer program HABIT. On the basis of the attachment energies of different crystal faces, the morphology was defined as {1 0 0}, {0 0 1}, {1 1 0}, {11bar0} and {1 01bar}. To confirm this theoretical prediction, we have grown ABP films and ABP crystals from the vapour phase. In both cases, the morphologically most important face was defined as {1 0 0} face using X-ray diffraction techniques. The remaining faces of the vapour-grown crystals were defined using a projection method, while the crystallites in the films were morphologically analysed by means of atomic force microscopy (AFM). The experimental morphologies are basically in agreement with the computation. Deviations from the equilibrium morphology can be ascribed to departure from equilibrium conditions during growth. For completeness, the results are compared with those for crystals grown from solutions for which deviations in morphology from the theoretical predictions can be ascribed to interaction between the crystal faces and solvent molecules.

Antibacterial Studies and Effect of Poloxamer on Gold Nanoparticles by Zingiber Officinale Extracted Green Synthesis.

PubMed

Chitra, K; Reena, K; Manikandan, A; Antony, S Arul

2015-07-01

Poloxamer finds excellent clinical and therapeutic uses for curing of various ailments. The Zin- giber officinale (Z. officinale) is one of the well-known medicinal plants. The poloxamer188 and the rhizome extract of Z. officinale have been used to synthesize the gold nanoparticles (AuNPs) by a green approach. The Z. officinale extract has been used as a reducing agent while the polox- amerl88 has been used as a stabilizing agent. The effect of addition of poloxamer on the controlling the shape and size of the AuNPs has been investigated by transmission electron microscopy (TEM) and dynamic light scattering techniques. The formation of AuNPs has also been confirmed by UV-Visible spectral, energy dispersive X-ray (EDX) and powder X-ray diffraction (XRD) analyses. The anti-bacterial activity of the green synthesized AuNPs has been investigated on the three human pathogens Staphylococcus aureus, Escherichia coli, and Klebsiella pneumonia. The poloxamer188 protected AuNPs inhibit the bacterial growth more effectively than the pure Z. officinale extract and the standard tetracycline (TA).

Color fluctuations in hadrons and proton coherent diffractive dissociation on helium

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

Strikman, M.; Guzey, V.

The differential cross section of inelastic coherent diffractive dissociation off nuclei {ital p}+{sup 4}He {r_arrow}{ital X}+{sup 4}He is expressed in terms of the relative cumulants of the cross-section distribution {ital P}{sub {ital N}}({sigma}). The theoretical result for the ratio {ital r}=({ital d}{sigma}{sub diff}/{ital dt}){sub {ital t}=0}{sup {ital p}He}/({ital d}{sigma}{sub diff}/{ital dt}) {sub {ital t}=0}{sup {ital pp}}=6.8--7.6 is close to the value {ital r}=7.1{plus_minus}0.7 which we extracted from the FNAL data. These are the only {ital A}{gt}2 data of this kind. The comparison provides the first confirmation of the color/cross-section fluctuation approach to the description of the absolute value of themore » inelastic diffraction cross section off nuclei. It provides also a new constraint on the first four cumulants of the cross-section distribution.« less

Quantifying point defects in Cu 2 ZnSn(S,Se) 4 thin films using resonant x-ray diffraction

DOE PAGES

Stone, Kevin H.; Christensen, Steven T.; Harvey, Steven P.; ...

2016-10-17

Cu 2ZnSn(S,Se)4 is an interesting, earth abundant photovoltaic material, but has suffered from low open circuit voltage. To better understand the film structure, we have measured resonant x-ray diffraction across the Cu and Zn K-edges for the device quality thin films of Cu 2ZnSnS4 (8.6% efficiency) and Cu 2ZnSn(S,Se)4 (3.5% efficiency). This approach allows for the confirmation of the underlying kesterite structure and quantification of the concentration of point defects and vacancies on the Cu, Zn, and Sn sublattices. Rietveld refinement of powder diffraction data collected at multiple energies is used to determine that there exists a high level ofmore » Cu Zn and Zn Cu defects on the 2c and 2d Wyckoff positions. We observe a significantly lower concentration of Zn Sn defects and Cu or Zn vacancies.« less

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

PubMed

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

2015-02-25

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

Amorphous tantala and its relationship with the molten state

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

Alderman, Oliver L.G.; Benmore, C. J.; Neuefeind, Joerg C.

The structure factors of molten Ta 2O 5 and Nb 2O 5 have been measured by high-energy x-ray and pulsed neutron diffraction. These are compared to transmission-mode x-ray diffraction through a self-supported 15-μm ion-beam sputtered amorphous tantala film. Atomistic models derived from the diffraction data by means of empirical potential structure refinement reveal that tantala and niobia liquids are very close to isomorphous, as confirmed by measurement of a molten mixture, Ta 0.8Nb 1.2O 5. Nonetheless, peak Nb-O bond lengths are about 1% shorter than those for Ta-O, at temperatures, T*=T/T melt, scaled to the melting points. Mean coordination numbersmore » are n MO≃5.6(1),n OM≃2.23(4) in the liquid state, and n TaO≃6.6(2),n OTa≃2.63(8) in the solid. The liquids are built from five- and six-fold M-O polyhedra which connect principally by corner sharing, with a minority of edge sharing; a-Ta 2O 5 on the other hand has a local structure more akin to the crystalline polymorphs, built primarily from six- and seven-fold polyhedra, with a larger degree of edge sharing. The structural differences between liquid and amorphous Ta 2O 5, coupled with observations of increasing peak bond lengths upon cooling, are consistent with the interpretation that the amorphous film reaches a supercooled liquidlike metastable equilibrium during deposition. In other words, the amorphous film shares a common progenitor state with a hypothetical glass quenched from a fragile melt. In addition, we show that recent classical interatomic potentials do not fully reproduce the diffraction data, and infer that inclusion of attractive (non-Coulombic) Ta-Ta interactions is important, particularly for obtaining the correct degree of edge sharing, coordination numbers, and densities. In conclusion, nanoscale inhomogeneity of the amorphous film is confirmed by the observation of small-angle x-ray scattering.« less

Formation of Fluorohydroxyapatite with Silver Diamine Fluoride

PubMed Central

Mei, M.L.; Nudelman, F.; Marzec, B.; Walker, J.M.; Lo, E.C.M.; Walls, A.W.; Chu, C.H.

2017-01-01

Silver diamine fluoride (SDF) is found to promote remineralization and harden the carious lesion. Hydroxyapatite crystallization is a crucial process in remineralization; however, the role of SDF in crystal formation is unknown. We designed an in vitro experiment with calcium phosphate with different SDF concentrations (0.38, 1.52, 2.66, 3.80 mg/mL) to investigate the effect of this additive on the nucleation and growth of apatite crystals. Two control groups were also prepared—calcium phosphate (CaCl2·2H2O + K2HPO4 in buffer solution) and SDF (Ag[NH3]2F in buffer solution). After incubation at 37 oC for 24 h, the shape and organization of the crystals were examined by bright-field transmission electron microscopy and electron diffraction. Unit cell parameters of the obtained crystals were determined with powder X-ray diffraction. The vibrational and rotational modes of phosphate groups were analyzed with Raman microscopy. The transmission electron microscopy and selected-area electron diffraction confirmed that all solids precipitated within the SDF groups were crystalline and that there was a positive correlation between the increased percentage of crystal size and the concentration of SDF. The powder X-ray diffraction patterns indicated that fluorohydroxyapatite and silver chloride were formed in all the SDF groups. Compared with calcium phosphate control, a contraction of the unit cell in the a-direction but not the c-direction in SDF groups was revealed, which suggested that small localized fluoride anions substituted the hydroxyl anions in hydroxyapatite crystals. This was further evidenced by the Raman spectra, which displayed up-field shift of the phosphate band in all the SDF groups and confirmed that the chemical environment of the phosphate functionalities indeed changed. The results suggested that SDF reacted with calcium and phosphate ions and produced fluorohydroxyapatite. This preferential precipitation of fluorohydroxyapatite with reduced solubility could be one of the main factors for arrest of caries lesions treated with SDF. PMID:28521107

Amorphous tantala and its relationship with the molten state

NASA Astrophysics Data System (ADS)

Alderman, O. L. G.; Benmore, C. J.; Neuefeind, J.; Coillet, E.; Mermet, A.; Martinez, V.; Tamalonis, A.; Weber, R.

2018-04-01

The structure factors of molten T a2O5 and N b2O5 have been measured by high-energy x-ray and pulsed neutron diffraction. These are compared to transmission-mode x-ray diffraction through a self-supported 15-μm ion-beam sputtered amorphous tantala film. Atomistic models derived from the diffraction data by means of empirical potential structure refinement reveal that tantala and niobia liquids are very close to isomorphous, as confirmed by measurement of a molten mixture, T a0.8N b1.2O5 . Nonetheless, peak Nb-O bond lengths are about 1 % shorter than those for Ta-O, at temperatures, T*=T /Tmelt , scaled to the melting points. Mean coordination numbers are nM O≃5.6 (1 ) ,nO M≃2.23 (4 ) in the liquid state, and nTaO≃6.6 (2 ) ,nOTa≃2.63 (8 ) in the solid. The liquids are built from five- and six-fold M -O polyhedra which connect principally by corner sharing, with a minority of edge sharing; a-T a2O5 on the other hand has a local structure more akin to the crystalline polymorphs, built primarily from six- and seven-fold polyhedra, with a larger degree of edge sharing. The structural differences between liquid and amorphous T a2O5 , coupled with observations of increasing peak bond lengths upon cooling, are consistent with the interpretation that the amorphous film reaches a supercooled liquidlike metastable equilibrium during deposition. In other words, the amorphous film shares a common progenitor state with a hypothetical glass quenched from a fragile melt. In addition, we show that recent classical interatomic potentials do not fully reproduce the diffraction data, and infer that inclusion of attractive (non-Coulombic) Ta-Ta interactions is important, particularly for obtaining the correct degree of edge sharing, coordination numbers, and densities. Nanoscale inhomogeneity of the amorphous film is confirmed by the observation of small-angle x-ray scattering.

Amorphous tantala and its relationship with the molten state

DOE PAGES

Alderman, Oliver L.G.; Benmore, C. J.; Neuefeind, Joerg C.; ...

2018-04-01

The structure factors of molten Ta 2O 5 and Nb 2O 5 have been measured by high-energy x-ray and pulsed neutron diffraction. These are compared to transmission-mode x-ray diffraction through a self-supported 15-μm ion-beam sputtered amorphous tantala film. Atomistic models derived from the diffraction data by means of empirical potential structure refinement reveal that tantala and niobia liquids are very close to isomorphous, as confirmed by measurement of a molten mixture, Ta 0.8Nb 1.2O 5. Nonetheless, peak Nb-O bond lengths are about 1% shorter than those for Ta-O, at temperatures, T*=T/T melt, scaled to the melting points. Mean coordination numbersmore » are n MO≃5.6(1),n OM≃2.23(4) in the liquid state, and n TaO≃6.6(2),n OTa≃2.63(8) in the solid. The liquids are built from five- and six-fold M-O polyhedra which connect principally by corner sharing, with a minority of edge sharing; a-Ta 2O 5 on the other hand has a local structure more akin to the crystalline polymorphs, built primarily from six- and seven-fold polyhedra, with a larger degree of edge sharing. The structural differences between liquid and amorphous Ta 2O 5, coupled with observations of increasing peak bond lengths upon cooling, are consistent with the interpretation that the amorphous film reaches a supercooled liquidlike metastable equilibrium during deposition. In other words, the amorphous film shares a common progenitor state with a hypothetical glass quenched from a fragile melt. In addition, we show that recent classical interatomic potentials do not fully reproduce the diffraction data, and infer that inclusion of attractive (non-Coulombic) Ta-Ta interactions is important, particularly for obtaining the correct degree of edge sharing, coordination numbers, and densities. In conclusion, nanoscale inhomogeneity of the amorphous film is confirmed by the observation of small-angle x-ray scattering.« less

Mode of action studies on the formation of enamel minerals from a novel toothpaste containing calcium silicate and sodium phosphate salts.

PubMed

Sun, Yuekui; Li, Xiaoke; Deng, Yan; Sun, Jianing N; Tao, DanYing; Chen, Hui; Hu, Qinghong; Liu, Renjiang; Liu, Weining; Feng, Xiping; Wang, Jinfang; Carvell, Mel; Joiner, Andrew

2014-06-01

To investigate in vitro and in situ the deposition and formation of hydroxyapatite (HAP) on enamel surfaces following brushing with a novel toothpaste containing calcium silicate (CaSi), sodium phosphate salts and fluoride. Polished enamel blocks were brushed in vitro with a slurry of the CaSi toothpaste. After one brush and four weeks simulated brushing the enamel surfaces were analysed. In an in situ protocol, enamel blocks were attached to first or second molar teeth of healthy subjects, exposed to 4 weeks twice per day brushing with the CaSi toothpaste and then analysed. The surface deposits were analysed using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). In addition, the CaSi toothpaste was slurried in simulated oral fluid (SOF) over a 3 hour period and the solids were isolated and analysed by Fourier transform infrared spectroscopy (FTIR). The FTIR study demonstrated that calcium phosphate phases had formed and these became increasingly crystalline over 3 hours. CaSi was deposited onto enamel surfaces following one brushing with the toothpaste in vitro.The deposited particles showed evidence of HAP crystalline phases associated with the CaSi. Following 4 weeks brushing in vitro, the deposition increased and analyses showed that the deposited material was HAP. These results were confirmed by the in situ study. Calcium silicate can be deposited onto enamel surfaces from a novel toothpaste formulation where it can form the enamel mineral HAP. A novel toothpaste formulation containing CaSi can form HAP on enamel surfaces. The potential of this technology is for a novel approach to the repair of demineralised enamel and the protection of enamel during acid exposure. © 2014 Elsevier Ltd. All rights reserved.

Endophytic synthesis of silver chloride nanoparticles from Penicillium sp. of Calophyllum apetalum

NASA Astrophysics Data System (ADS)

Chandrappa, C. P.; Govindappa, M.; Chandrasekar, N.; Sarkar, Sonia; Ooha, Sepuri; Channabasava, R.

2016-06-01

In the present study, Penicillium species extract isolated from Calophyllum apetalum was used for the synthesis of silver nanoparticles and it was confirmed by changing the color of the silver nitrate UV-Vis spectrum. The synthesized nanoparticles have been characterized by biophysical techniques such as scanning electron microscopy and x-ray diffraction.

Nucleation kinetics of urea succinic acid –ferroelectric single crystal

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

Dhivya, R.; Voohrees College, Vellore-632014, Tamilnadu; Vizhi, R. Ezhil, E-mail: rezhilvizhi@vit.ac.in, E-mail: revizhi@gmail.com

2015-06-24

Single crystals of Urea Succinic Acid (USA) were grown by slow cooling technique. The crystalline system was confirmed by powder X-ray diffraction. The metastable zonewidth were carried out for various temperatures i.e., 35°, 40°, 45° and 50°C. The induction period is experimentally determined and various nucleation parameters have been estimated.

Higher value films prepared from poly(vinyl alcohol) and amylose-fatty acid derivatives inclusion complexes

USDA-ARS?s Scientific Manuscript database

Water soluble amylose fatty acid and fatty ammonium salt inclusion complexes (AIC) were prepared by jet cooked high amylose corn starch with water soluble salts of long chain fatty acids or fatty amines. The formation of AIC was confirmed by X-ray diffraction of freeze-dried samples. After dissoluti...

Reaction layer formation at the graphite/copper-chromium alloy interface

NASA Technical Reports Server (NTRS)

Devincent, Sandra M.; Michal, Gary M.

1992-01-01

Sessile drop tests were used to obtain information about copper chromium alloys that suitably wet graphite. Characterization of graphite/copper-chromium alloy interfaces subjected to elevated temperatures were conducted using scanning electron micrography, energy dispersive spectroscopy, auger electron spectroscopy, and x ray diffraction analyses. These analyses indicate that during sessile drop tests conducted at 1130 C for one hour, copper alloys containing greater than 0.98 percent chromium form continuous reaction layers of approximately 10 micron thickness. The reaction layers adhere to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 degrees or less. X ray diffraction results indicate that the reaction layer is chromium carbide. The kinetics of reaction layer formation were modelled in terms of bulk diffusion mechanisms. Reaction layer thickness is controlled initially by the diffusion of Cr out of Cu alloy and later by the diffusion of C through chromium carbide.

Reaction layer formation at the graphite/copper-chromium alloy interface

NASA Technical Reports Server (NTRS)

Devincent, Sandra M.; Michal, Gary M.

1993-01-01

Sessile drop tests were used to obtain information about copper chromium alloys that suitably wet graphite. Characterization of graphite/copper-chromium alloy interfaces subjected to elevated temperatures were conducted using scanning electron micrography, energy dispersive spectroscopy, Auger electron spectroscopy, and X-ray diffraction analyses. These analyses indicate that during sessile drop tests conducted at 1130 C for one hour, copper alloys containing greater than 0.98 percent chromium form continuous reaction layers of approximately 10 micron thickness. The reaction layers adhere to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 degrees or less. X-ray diffraction results indicate that the reaction layer is chromium carbide. The kinetics of reaction layer formation were modelled in terms of bulk diffusion mechanisms. Reaction layer thickness is controlled initially by the diffusion of Cr out of Cu alloy and later by the diffusion of C through chromium carbide.

The structure of denisovite, a fibrous nanocrystalline polytypic disordered ‘very complex’ silicate, studied by a synergistic multi-disciplinary approach employing methods of electron crystallography and X-ray powder diffraction

PubMed Central

Schowalter, Marco; Schmidt, Martin U.; Czank, Michael; Depmeier, Wulf; Rosenauer, Andreas

2017-01-01

Denisovite is a rare mineral occurring as aggregates of fibres typically 200–500 nm diameter. It was confirmed as a new mineral in 1984, but important facts about its chemical formula, lattice parameters, symmetry and structure have remained incompletely known since then. Recently obtained results from studies using microprobe analysis, X-ray powder diffraction (XRPD), electron crystallography, modelling and Rietveld refinement will be reported. The electron crystallography methods include transmission electron microscopy (TEM), selected-area electron diffraction (SAED), high-angle annular dark-field imaging (HAADF), high-resolution transmission electron microscopy (HRTEM), precession electron diffraction (PED) and electron diffraction tomography (EDT). A structural model of denisovite was developed from HAADF images and later completed on the basis of quasi-kinematic EDT data by ab initio structure solution using direct methods and least-squares refinement. The model was confirmed by Rietveld refinement. The lattice parameters are a = 31.024 (1), b = 19.554 (1) and c = 7.1441 (5) Å, β = 95.99 (3)°, V = 4310.1 (5) Å3 and space group P12/a1. The structure consists of three topologically distinct dreier silicate chains, viz. two xonotlite-like dreier double chains, [Si6O17]10−, and a tubular loop-branched dreier triple chain, [Si12O30]12−. The silicate chains occur between three walls of edge-sharing (Ca,Na) octahedra. The chains of silicate tetrahedra and the octahedra walls extend parallel to the z axis and form a layer parallel to (100). Water molecules and K+ cations are located at the centre of the tubular silicate chain. The latter also occupy positions close to the centres of eight-membered rings in the silicate chains. The silicate chains are geometrically constrained by neighbouring octahedra walls and present an ambiguity with respect to their z position along these walls, with displacements between neighbouring layers being either Δz = c/4 or −c/4. Such behaviour is typical for polytypic sequences and leads to disorder along [100]. In fact, the diffraction pattern does not show any sharp reflections with l odd, but continuous diffuse streaks parallel to a* instead. Only reflections with l even are sharp. The diffuse scattering is caused by (100) nano­lamellae separated by stacking faults and twin boundaries. The structure can be described according to the order–disorder (OD) theory as a stacking of layers parallel to (100). PMID:28512570

Quality Assessment of Urinary Stone Analysis: Results of a Multicenter Study of Laboratories in Europe

PubMed Central

Siener, Roswitha; Buchholz, Noor; Daudon, Michel; Hess, Bernhard; Knoll, Thomas; Osther, Palle J.; Reis-Santos, José; Sarica, Kemal; Traxer, Olivier; Trinchieri, Alberto

2016-01-01

After stone removal, accurate analysis of urinary stone composition is the most crucial laboratory diagnostic procedure for the treatment and recurrence prevention in the stone-forming patient. The most common techniques for routine analysis of stones are infrared spectroscopy, X-ray diffraction and chemical analysis. The aim of the present study was to assess the quality of urinary stone analysis of laboratories in Europe. Nine laboratories from eight European countries participated in six quality control surveys for urinary calculi analyses of the Reference Institute for Bioanalytics, Bonn, Germany, between 2010 and 2014. Each participant received the same blinded test samples for stone analysis. A total of 24 samples, comprising pure substances and mixtures of two or three components, were analysed. The evaluation of the quality of the laboratory in the present study was based on the attainment of 75% of the maximum total points, i.e. 99 points. The methods of stone analysis used were infrared spectroscopy (n = 7), chemical analysis (n = 1) and X-ray diffraction (n = 1). In the present study only 56% of the laboratories, four using infrared spectroscopy and one using X-ray diffraction, fulfilled the quality requirements. According to the current standard, chemical analysis is considered to be insufficient for stone analysis, whereas infrared spectroscopy or X-ray diffraction is mandatory. However, the poor results of infrared spectroscopy highlight the importance of equipment, reference spectra and qualification of the staff for an accurate analysis of stone composition. Regular quality control is essential in carrying out routine stone analysis. PMID:27248840

Quality Assessment of Urinary Stone Analysis: Results of a Multicenter Study of Laboratories in Europe.

PubMed

Siener, Roswitha; Buchholz, Noor; Daudon, Michel; Hess, Bernhard; Knoll, Thomas; Osther, Palle J; Reis-Santos, José; Sarica, Kemal; Traxer, Olivier; Trinchieri, Alberto

2016-01-01

After stone removal, accurate analysis of urinary stone composition is the most crucial laboratory diagnostic procedure for the treatment and recurrence prevention in the stone-forming patient. The most common techniques for routine analysis of stones are infrared spectroscopy, X-ray diffraction and chemical analysis. The aim of the present study was to assess the quality of urinary stone analysis of laboratories in Europe. Nine laboratories from eight European countries participated in six quality control surveys for urinary calculi analyses of the Reference Institute for Bioanalytics, Bonn, Germany, between 2010 and 2014. Each participant received the same blinded test samples for stone analysis. A total of 24 samples, comprising pure substances and mixtures of two or three components, were analysed. The evaluation of the quality of the laboratory in the present study was based on the attainment of 75% of the maximum total points, i.e. 99 points. The methods of stone analysis used were infrared spectroscopy (n = 7), chemical analysis (n = 1) and X-ray diffraction (n = 1). In the present study only 56% of the laboratories, four using infrared spectroscopy and one using X-ray diffraction, fulfilled the quality requirements. According to the current standard, chemical analysis is considered to be insufficient for stone analysis, whereas infrared spectroscopy or X-ray diffraction is mandatory. However, the poor results of infrared spectroscopy highlight the importance of equipment, reference spectra and qualification of the staff for an accurate analysis of stone composition. Regular quality control is essential in carrying out routine stone analysis.

Gold nanoparticles interacting with β-cyclodextrin-phenylethylamine inclusion complex: a ternary system for photothermal drug release.

PubMed

Sierpe, Rodrigo; Lang, Erika; Jara, Paul; Guerrero, Ariel R; Chornik, Boris; Kogan, Marcelo J; Yutronic, Nicolás

2015-07-22

We report the synthesis of a 1:1 β-cyclodextrin-phenylethylamine (βCD-PhEA) inclusion complex (IC) and the adhesion of gold nanoparticles (AuNPs) onto microcrystals of this complex, which forms a ternary system. The formation of the IC was confirmed by powder X-ray diffraction and NMR analyses ((1)H and ROESY). The stability constant of the IC (760 M(-1)) was determined using the phase solubility method. The adhesion of AuNPs was obtained using the magnetron sputtering technique, and the presence of AuNPs was confirmed using UV-vis spectroscopy (surface plasmon resonance effect), which showed an absorbance at 533 nm. The powder X-ray diffractograms of βCD-PhEA were similar to those of the crystals decorated with AuNPs. A comparison of the one- and two-dimensional NMR spectra of the IC with and without AuNPs suggests partial displacement of the guest to the outside of the βCD due to attraction toward AuNPs, a characteristic tropism effect. The size, morphology, and distribution of the AuNPs were analyzed using TEM and SEM. The average size of the AuNPs was 14 nm. Changes in the IR and Raman spectra were attributed to the formation of the complex and to the specific interactions of this group with the AuNPs. Laser irradiation assays show that the ternary system βCD-PhEA-AuNPs in solution enables the release of the guest.

Fabrication and characterization of novel multilayered structures by stereocomplexion of poly(D-lactic acid)/poly(L-lactic acid) and self-assembly of polyelectrolytes.

PubMed

Dellacasa, Elena; Zhao, Li; Yang, Gesheng; Pastorino, Laura; Sukhorukov, Gleb B

2016-01-01

The enantiomers poly(D-lactic acid) (PDLA) and poly(L-lactic acid) (PLLA) were alternately adsorbed directly on calcium carbonate (CaCO3) templates and on poly(styrene sulfonate) (PSS) and poly(allylamine hydrochloride) (PAH) multilayer precursors in order to fabricate a novel layer-by-layer (LBL) assembly. A single layer of poly(L-lysine) (PLL) was used as a linker between the (PDLA/PLLA) n stereocomplex and the cores with and without the polymeric (PSS/PAH) n /PLL multilayer precursor (PEM). Nuclear magnetic resonance (NMR) and gel permeation chromatography (GPC) were used to characterize the chemical composition and molecular weight of poly(lactic acid) polymers. Both multilayer structures, with and without polymeric precursor, were firstly fabricated and characterized on planar supports. A quartz crystal microbalance (QCM), attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) and ellipsometry were used to evaluate the thickness and mass of the multilayers. Then, hollow, spherical microcapsules were obtained by the removal of the CaCO3 sacrificial template. The chemical composition of the obtained microcapsules was confirmed by differential scanning calorimetry (DSC) and wide X-ray diffraction (WXRD) analyses. The microcapsule morphology was evaluated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) measurements. The experimental results confirm the successful fabrication of this innovative system, and its full biocompatibility makes it worthy of further characterization as a promising drug carrier for sustained release.

Fabrication and characterization of novel multilayered structures by stereocomplexion of poly(D-lactic acid)/poly(L-lactic acid) and self-assembly of polyelectrolytes

PubMed Central

Yang, Gesheng; Pastorino, Laura

2016-01-01

Summary The enantiomers poly(D-lactic acid) (PDLA) and poly(L-lactic acid) (PLLA) were alternately adsorbed directly on calcium carbonate (CaCO3) templates and on poly(styrene sulfonate) (PSS) and poly(allylamine hydrochloride) (PAH) multilayer precursors in order to fabricate a novel layer-by-layer (LBL) assembly. A single layer of poly(L-lysine) (PLL) was used as a linker between the (PDLA/PLLA)n stereocomplex and the cores with and without the polymeric (PSS/PAH)n/PLL multilayer precursor (PEM). Nuclear magnetic resonance (NMR) and gel permeation chromatography (GPC) were used to characterize the chemical composition and molecular weight of poly(lactic acid) polymers. Both multilayer structures, with and without polymeric precursor, were firstly fabricated and characterized on planar supports. A quartz crystal microbalance (QCM), attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) and ellipsometry were used to evaluate the thickness and mass of the multilayers. Then, hollow, spherical microcapsules were obtained by the removal of the CaCO3 sacrificial template. The chemical composition of the obtained microcapsules was confirmed by differential scanning calorimetry (DSC) and wide X-ray diffraction (WXRD) analyses. The microcapsule morphology was evaluated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) measurements. The experimental results confirm the successful fabrication of this innovative system, and its full biocompatibility makes it worthy of further characterization as a promising drug carrier for sustained release. PMID:26925356

Tuning the morphology of metastable MnS films by simple chemical bath deposition technique

NASA Astrophysics Data System (ADS)

Dhandayuthapani, T.; Girish, M.; Sivakumar, R.; Sanjeeviraja, C.; Gopalakrishnan, R.

2015-10-01

In the present investigation, we have prepared the spherical particles, almond-like, and cauliflower-like morphological structures of metastable MnS films on glass substrate by chemical bath deposition technique at low temperature without using any complexing or chelating agent. The morphological change of MnS films with molar ratio may be due to the oriented aggregation of adjacent particles. The compositional purity of deposited film was confirmed by the EDAX study. X-ray diffraction and micro-Raman studies confirm the sulfur source concentration induced enhancement in the crystallization of films with metastable MnS phase (zinc-blende β-MnS, and wurtzite γ-MnS). The shift in PL emission peak with molar ratio may be due to the change in optical energy band gap of the MnS, which was further confirmed by the optical absorbance study. The paramagnetic behavior of the sample was confirmed by the M-H plot.

Structural, Optical, and Vibrational Properties of ZnO Microrods Deposited on Silicon Substrate

NASA Astrophysics Data System (ADS)

Lahlouh, Bashar I.; Ikhmayies, Shadia J.; Juwhari, Hassan K.

2018-03-01

Zinc oxide (ZnO) microrod films deposited by spray pyrolysis on silicon substrate at 350 ± 5°C have been studied and evaluated, and compared with thin films deposited by electron beam to confirm the identity of the studied samples. The films were characterized using different techniques. The microrod structure was studied and confirmed by scanning electron microscopy. Fourier-transform infrared (FTIR) spectroscopy and x-ray diffraction analysis confirmed successful deposition of ZnO thin films with the expected wurtzite structure. Reflectance data showed a substantial drop across the whole studied wavelength range. The photoluminescence (PL) spectra of the studied samples showed a peak at ˜ 360 nm, representing a signature of ZnO. The shift in the PL peak position is due to defects and other species present in the films, as confirmed by FTIR and energy-dispersive x-ray spectroscopy results.

HR-EBSD as a new tool for quantifying geometrically necessary dislocations in quartz: Application to chessboard subgrain boundaries

NASA Astrophysics Data System (ADS)

Wallis, D.; Parsons, A. J.; Hansen, L. N.

2017-12-01

Chessboard subgrains in quartz, with boundaries composed of {m}[c] edge dislocations, are widely used as evidence for high-temperature deformation and have been suggested to form only in β-quartz. However, the origins and dislocation structure of chessboard subgrains remain poorly constrained and, without precise constraints on axes of misorientations across subgrain boundaries, other subgrain types formed at lower temperatures can be misidentified as chessboard subgrains. The technique most commonly employed to investigate subgrain structures, electron backscatter diffraction, can only resolve misorientation angles and axes for a portion of the substructure. This limitation hinders detailed interpretation of the dislocation types, densities, and processes that generate characteristic subgrain structures. We overcome these limitations by employing high-angular resolution electron backscatter diffraction (HR-EBSD), which employs cross-correlation of diffraction patterns to achieve angular resolution on the order of 0.01° with well-constrained misorientation axes. We analyse chessboard subgrains in samples from the Greater Himalayan Sequence, Nepal, which were deformed along well constrained pressure-temperature paths confined to the stability field of α-quartz. HR-EBSD analysis demonstrates that the subgrain boundaries consist of two sets. One set consists primarily of {m}[c] edge dislocations and the other consists of dislocations primarily with Burgers vectors. Apparent densities of geometrically necessary dislocations vary from > 1013 m-2 within some subgrain boundaries to < 1012 m-2 within subgrain interiors. This analysis provides new insight into the structure of chessboard subgrain boundaries, and a new tool to distinguish them from superficially similar deformation microstructures formed by other dislocation types at lower temperatures. Application of HR-EBSD to quartz from the Greater Himalayan Sequence confirms the activity of {m}[c] slip in the α-quartz stability field and demonstrates that formation of chessboard subgrains is not restricted to the stability field of β-quartz. Most importantly, this study demonstrates the potential of HR-EBSD as an improved method for analysis of quartz microstructures used as indicators of deformation conditions.

Strongly coupled electronic, magnetic, and lattice degrees of freedom in LaCo 5 under pressure

DOE PAGES

Stillwell, Ryan L.; Jeffries, Jason R.; McCall, Scott K.; ...

2015-11-25

In this study, we have performed high-pressure magnetotransport and x-ray diffraction measurements on ferromagnetic LaCo 5, confirming the theoretically predicted electronic topological transition driving the magnetoelastic collapse seen in the related compound YCo 5. Our x-ray diffraction results show an anisotropic lattice collapse of the c axis near 10 GPa that is also commensurate with a change in the majority charge carriers evident from high-pressure Hall effect measurements. The coupling of the electronic, magnetic, and lattice degrees of freedom is further substantiated by the evolution of the anomalous Hall effect, which couples to the magnetization of the ordered state ofmore » LaCo 5.« less

Structural and spectral properties of MgZnO2:Sm3+ phosphor

NASA Astrophysics Data System (ADS)

Rajput, Preasha; Sharma, Pallavi; Biswas, Pankaj; Kamni

2018-05-01

The samarium doped MgZnO2 phosphor was synthesized by the low-cost combustion method. The powder X-ray diffraction (XRD) analysis confirmed the crystallinity and phase purity of the phosphor. The lattice parameters were determined by indexing the diffraction peaks. The photoluminescence (PL) study revealed that the phosphor exhibited a broad excitation band in the UV region ranging between 200 to 350 nm. The 601 nm emission was ascribed to 4G5/2 to 6H7/2 transitions of the Sm3+ ion. The optical bandgap of MgZnO2:Sm3+ was obtained to be 3.56 eV. The phosphor can be projected as a useful material in X- and gamma-ray scintillators.

Direct observation of anti-phase boundaries in heteroepitaxy of GaSb thin films grown on Si(001) by transmission electron microscopy

NASA Astrophysics Data System (ADS)

Woo, S. Y.; Hosseini Vajargah, S.; Ghanad-Tavakoli, S.; Kleiman, R. N.; Botton, G. A.

2012-10-01

Unambiguous identification of anti-phase boundaries (APBs) in heteroepitaxial films of GaSb grown on Si has been so far elusive. In this work, we present conventional transmission electron microscopy (TEM) diffraction contrast imaging using superlattice reflections, in conjunction with convergent beam electron diffraction analysis, to determine a change in polarity across APBs in order to confirm the presence of anti-phase disorder. In-depth analysis of anti-phase disorder is further supported with atomic resolution high-angle annular dark-field scanning transmission electron microscopy. The nature of APBs in GaSb is further elucidated by a comparison to previous results for GaAs epilayers grown on Si.

Nanocrystalline NiNd{sub 0.01}Fe{sub 1.99}O{sub 4} as a gas sensor

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

Shinde, Tukaram J., E-mail: pshindetj@yahoo.co.in; Gadkari, Ashok B.; Jadhav, Sarjerao R.

2015-06-24

Nanocrystalline NiNd{sub 0.01}Fe{sub 1.99}O{sub 4} has been synthesized by oxalate co-precipitation method and was characterized by X-ray diffraction technique. X-ray diffraction analysis confirms the formation of single phase cubic spinel structure. Crystallite size of the ferrite lies in the nano-particle range. The gas sensing properties of nanocrystalline ferrite were studied for gases like Cl{sub 2}, LPG and C{sub 2}H{sub 5}OH. It was observed that NiNd{sub 0.01}Fe{sub 1.99}O{sub 4} is more sensitive towards chlorine followed by LPG at an operating temperature 277 °C compared to ethanol.

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

Tumurugoti, P.; Clark, B.M.; Edwards, D.J.

Hollandite-rich multiphase waste form compositions processed by melt-solidification and spark plasma sintering (SPS) were characterized, compared, and validated for nuclear waste incorporation. Phase identification by x-ray diffraction (XRD) and electron back-scattered diffraction (EBSD) confirmed hollandite as the major phase present in these samples along with perovskite, pyrochlore and zirconolite. Distribution of selected elements observed by wavelength dispersive spectroscopy (WDS) maps indicated that Cs formed a secondary phase during SPS processing, which was considered undesirable. On the other hand, Cs partitioned into the hollandite phase in melt-processed samples. Further analysis of hollandite structure in melt-processed composition by selected area electron diffractionmore » (SAED) revealed ordered arrangement of tunnel ions (Ba/Cs) and vacancies, suggesting efficient Cs incorporation into the lattice.« less

The magnetic order of GdMn₂Ge₂ studied by neutron diffraction and x-ray resonant magnetic scattering.

PubMed

Granovsky, S A; Kreyssig, A; Doerr, M; Ritter, C; Dudzik, E; Feyerherm, R; Canfield, P C; Loewenhaupt, M

2010-06-09

The magnetic structure of GdMn₂Ge₂ (tetragonal I4/mmm) has been studied by hot neutron powder diffraction and x-ray resonant magnetic scattering techniques. These measurements, along with the results of bulk experiments, confirm the collinear ferrimagnetic structure with moment direction parallel to the c-axis below T(C) = 96 K and the collinear antiferromagnetic phase in the temperature region T(C) < T < T(N) = 365 K. In the antiferromagnetic phase, x-ray resonant magnetic scattering has been detected at Mn K and Gd L₂ absorption edges. The Gd contribution is a result of an induced Gd 5d electron polarization caused by the antiferromagnetic order of Mn-moments.

Sensitivity and Limitations of Structures from X-ray and Neutron-Based Diffraction Analyses of Transition Metal Oxide Lithium-Battery Electrodes

DOE PAGES

Liu, Hao; Liu, Haodong; Lapidus, Saul H.; ...

2017-06-21

Lithium transition metal oxides are an important class of electrode materials for lithium-ion batteries. Binary or ternary (transition) metal doping brings about new opportunities to improve the electrode’s performance and often leads to more complex stoichiometries and atomic structures than the archetypal LiCoO 2. Rietveld structural analyses of X-ray and neutron diffraction data is a widely-used approach for structural characterization of crystalline materials. But, different structural models and refinement approaches can lead to differing results, and some parameters can be difficult to quantify due to the inherent limitations of the data. Here, through the example of LiNi 0.8Co 0.15Al 0.05Omore » 2 (NCA), we demonstrated the sensitivity of various structural parameters in Rietveld structural analysis to different refinement approaches and structural models, and proposed an approach to reduce refinement uncertainties due to the inexact X-ray scattering factors of the constituent atoms within the lattice. Furthermore, this refinement approach was implemented for electrochemically-cycled NCA samples and yielded accurate structural parameters using only X-ray diffraction data. The present work provides the best practices for performing structural refinement of lithium transition metal oxides.« less

Sensitivity and Limitations of Structures from X-ray and Neutron-Based Diffraction Analyses of Transition Metal Oxide Lithium-Battery Electrodes

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

Liu, Hao; Liu, Haodong; Lapidus, Saul H.

Lithium transition metal oxides are an important class of electrode materials for lithium-ion batteries. Binary or ternary (transition) metal doping brings about new opportunities to improve the electrode’s performance and often leads to more complex stoichiometries and atomic structures than the archetypal LiCoO 2. Rietveld structural analyses of X-ray and neutron diffraction data is a widely-used approach for structural characterization of crystalline materials. But, different structural models and refinement approaches can lead to differing results, and some parameters can be difficult to quantify due to the inherent limitations of the data. Here, through the example of LiNi 0.8Co 0.15Al 0.05Omore » 2 (NCA), we demonstrated the sensitivity of various structural parameters in Rietveld structural analysis to different refinement approaches and structural models, and proposed an approach to reduce refinement uncertainties due to the inexact X-ray scattering factors of the constituent atoms within the lattice. Furthermore, this refinement approach was implemented for electrochemically-cycled NCA samples and yielded accurate structural parameters using only X-ray diffraction data. The present work provides the best practices for performing structural refinement of lithium transition metal oxides.« less

Advanced Structural Analyses by Third Generation Synchrotron Radiation Powder Diffraction

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

Sakata, M.; Aoyagi, S.; Ogura, T.

2007-01-19

Since the advent of the 3rd generation Synchrotron Radiation (SR) sources, such as SPring-8, the capabilities of SR powder diffraction increased greatly not only in an accurate structure refinement but also ab initio structure determination. In this study, advanced structural analyses by 3rd generation SR powder diffraction based on the Large Debye-Scherrer camera installed at BL02B2, SPring-8 is described. Because of high angular resolution and high counting statistics powder data collected at BL02B2, SPring-8, ab initio structure determination can cope with a molecular crystals with 65 atoms including H atoms. For the structure refinements, it is found that a kindmore » of Maximum Entropy Method in which several atoms are omitted in phase calculation become very important to refine structural details of fairy large molecule in a crystal. It should be emphasized that until the unknown structure is refined very precisely, the obtained structure by Genetic Algorithm (GA) or some other ab initio structure determination method using real space structural knowledge, it is not possible to tell whether the structure obtained by the method is correct or not. In order to determine and/or refine crystal structure of rather complicated molecules, we cannot overemphasize the importance of the 3rd generation SR sources.« less

Biogenic silver nanoparticles: efficient and effective antifungal agents

NASA Astrophysics Data System (ADS)

Netala, Vasudeva Reddy; Kotakadi, Venkata Subbaiah; Domdi, Latha; Gaddam, Susmila Aparna; Bobbu, Pushpalatha; Venkata, Sucharitha K.; Ghosh, Sukhendu Bikash; Tartte, Vijaya

2016-04-01

Biogenic synthesis of silver nanoparticles (AgNPs) by exploiting various plant materials is an emerging field and considered green nanotechnology as it involves simple, cost effective and ecofriendly procedure. In the present study AgNPs were successfully synthesized using aqueous callus extract of Gymnema sylvestre. The aqueous callus extract treated with 1nM silver nitrate solution resulted in the formation of AgNPs and the surface plasmon resonance (SPR) of the formed AgNPs showed a peak at 437 nm in the UV Visible spectrum. The synthesized AgNPs were characterized using Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), and X-ray diffraction spectroscopy (XRD). FTIR spectra showed the peaks at 3333, 2928, 2361, 1600, 1357 and 1028 cm-1 which revealed the role of different functional groups possibly involved in the synthesis and stabilization of AgNPs. TEM micrograph clearly revealed the size of the AgNPs to be in the range of 3-30 nm with spherical shape and poly-dispersed nature; it is further confirmed by Particle size analysis that the stability of AgNPs is due its high negative Zeta potential (-36.1 mV). XRD pattern revealed the crystal nature of the AgNPs by showing the braggs peaks corresponding to (111), (200), (220) and (311) planes of face-centered cubic crystal phase of silver. Selected area electron diffraction pattern showed diffraction rings and confirmed the crystalline nature of synthesized AgNPs. The synthesized AgNPs exhibited effective antifungal activity against Candida albicans, Candida nonalbicans and Candida tropicalis.

Scattering of S waves diffracted at the core-mantle boundary: forward modelling

NASA Astrophysics Data System (ADS)

Emery, Valérie; Maupin, Valérie; Nataf, Henri-Claude

1999-11-01

The lowermost 200-300 km of the Earth's mantle, known as the D'' layer, is an extremely complex and heterogeneous region where transfer processes between the core and the mantle take place. Diffracted S waves propagate over large distances and are very sensitive to the velocity structure of this region. Strong variations of ampli-tudes and waveforms are observed on recordings from networks of broad-band seismic stations. We perform forward modelling of diffracted S waves in laterally heterogeneous structures in order to analyse whether or not these observations can be related to lateral inhomogeneities in D''. We combine the diffraction due to the core and the scattering due to small-scale volumetric heterogeneities (10-100 km) by coupling single scattering (Born approximation) with the Langer approximation, which describes Sdiff wave propagation. The influence on the direct as well as on the scattered wavefields of the CMB as well as of possible tunnelling in the core or in D'' is fully accounted for. The SH and the SV components of the diffracted waves are analysed, as well as their coupling. The modelling is applied in heterogeneous models with different geometries: isolated heterogeneities, vertical cylinders, horizontal inhomogeneities and random media. Amplitudes of scattered waves are weak and only velocity perturbations of the order of 10 per cent over a volume of 240 x 240 x 300 km3 produce visible effects on seismograms. The two polarizations of Sdiff have different radial sensitivities, the SH components being more sensitive to heterogeneities closer to the CMB. However, we do not observe significant time-shifts between the two components similar to those produced by anisotropy. The long-period Sdiff have a poor lateral resolution and average the velocity perturbations in their Fresnel zone. Random small-scale heterogeneities with +/- 10 per cent velocity contrast in the layer therefore have little effect on Sdiff, in contrast to their effect on PKIKP.

High-resolution three-dimensional imaging of red blood cells parasitized by Plasmodium falciparum and in situ hemozoin crystals using optical diffraction tomography

NASA Astrophysics Data System (ADS)

Kim, Kyoohyun; Yoon, HyeOk; Diez-Silva, Monica; Dao, Ming; Dasari, Ramachandra R.; Park, YongKeun

2014-01-01

We present high-resolution optical tomographic images of human red blood cells (RBC) parasitized by malaria-inducing Plasmodium falciparum (Pf)-RBCs. Three-dimensional (3-D) refractive index (RI) tomograms are reconstructed by recourse to a diffraction algorithm from multiple two-dimensional holograms with various angles of illumination. These 3-D RI tomograms of Pf-RBCs show cellular and subcellular structures of host RBCs and invaded parasites in fine detail. Full asexual intraerythrocytic stages of parasite maturation (ring to trophozoite to schizont stages) are then systematically investigated using optical diffraction tomography algorithms. These analyses provide quantitative information on the structural and chemical characteristics of individual host Pf-RBCs, parasitophorous vacuole, and cytoplasm. The in situ structural evolution and chemical characteristics of subcellular hemozoin crystals are also elucidated.

How to make deposition of images a reality

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

Guss, J. Mitchell, E-mail: mitchell.guss@sydney.edu.au; McMahon, Brian; School of Molecular Bioscience, The University of Sydney, Sydney, NSW 2006

2014-10-01

An analysis is performed of the technical and financial challenges to be overcome if deposition of primary experimental data is to become routine. The IUCr Diffraction Data Deposition Working Group is investigating the rationale and policies for routine deposition of diffraction images (and other primary experimental data sets). An information-management framework is described that should inform policy directions, and some of the technical and other issues that need to be addressed in an effort to achieve such a goal are analysed. In the near future, routine data deposition could be encouraged at one of the growing number of institutional repositoriesmore » that accept data sets or at a generic data-publishing web repository service. To realise all of the potential benefits of depositing diffraction data, specialized archives would be preferable. Funding such an initiative will be challenging.« less

High-resolution three-dimensional imaging of red blood cells parasitized by Plasmodium falciparum and in situ hemozoin crystals using optical diffraction tomography

PubMed Central

Kim, Kyoohyun; Yoon, HyeOk; Diez-Silva, Monica; Dao, Ming; Dasari, Ramachandra R.

2013-01-01

Abstract. We present high-resolution optical tomographic images of human red blood cells (RBC) parasitized by malaria-inducing Plasmodium falciparum (Pf)-RBCs. Three-dimensional (3-D) refractive index (RI) tomograms are reconstructed by recourse to a diffraction algorithm from multiple two-dimensional holograms with various angles of illumination. These 3-D RI tomograms of Pf-RBCs show cellular and subcellular structures of host RBCs and invaded parasites in fine detail. Full asexual intraerythrocytic stages of parasite maturation (ring to trophozoite to schizont stages) are then systematically investigated using optical diffraction tomography algorithms. These analyses provide quantitative information on the structural and chemical characteristics of individual host Pf-RBCs, parasitophorous vacuole, and cytoplasm. The in situ structural evolution and chemical characteristics of subcellular hemozoin crystals are also elucidated. PMID:23797986

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

PubMed

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

2007-05-01

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

Coherent X-ray diffraction from collagenous soft tissues

PubMed Central

Berenguer de la Cuesta, Felisa; Wenger, Marco P. E.; Bean, Richard J.; Bozec, Laurent; Horton, Michael A.; Robinson, Ian K.

2009-01-01

Coherent X-ray diffraction has been applied in the imaging of inorganic materials with great success. However, its application to biological specimens has been limited to some notable exceptions, due to the induced radiation damage and the extended nature of biological samples, the last limiting the application of most part of the phasing algorithms. X-ray ptychography, still under development, is a good candidate to overcome such difficulties and become a powerful imaging method for biology. We describe herein the feasibility of applying ptychography to the imaging of biological specimens, in particular collagen rich samples. We report here speckles in diffraction patterns from soft animal tissue, obtained with an optimized small angle X-ray setup that exploits the natural coherence of the beam. By phasing these patterns, dark field images of collagen within tendon, skin, bone, or cornea will eventually be obtained with a resolution of 60–70 nm. We present simulations of the contrast mechanism in collagen based on atomic force microscope images of the samples. Simulations confirmed the ‘speckled’ nature of the obtained diffraction patterns. Once inverted, the patterns will show the disposition and orientation of the fibers within the tissue, by enhancing the phase contrast between protein and no protein regions of the sample. Our work affords the application of the most innovative coherent X-ray diffraction tools to the study of biological specimens, and this approach will have a significant impact in biology and medicine because it overcomes many of the limits of current microscopy techniques. PMID:19706395

Coherent X-ray diffraction from collagenous soft tissues.

PubMed

Berenguer de la Cuesta, Felisa; Wenger, Marco P E; Bean, Richard J; Bozec, Laurent; Horton, Michael A; Robinson, Ian K

2009-09-08

Coherent X-ray diffraction has been applied in the imaging of inorganic materials with great success. However, its application to biological specimens has been limited to some notable exceptions, due to the induced radiation damage and the extended nature of biological samples, the last limiting the application of most part of the phasing algorithms. X-ray ptychography, still under development, is a good candidate to overcome such difficulties and become a powerful imaging method for biology. We describe herein the feasibility of applying ptychography to the imaging of biological specimens, in particular collagen rich samples. We report here speckles in diffraction patterns from soft animal tissue, obtained with an optimized small angle X-ray setup that exploits the natural coherence of the beam. By phasing these patterns, dark field images of collagen within tendon, skin, bone, or cornea will eventually be obtained with a resolution of 60-70 nm. We present simulations of the contrast mechanism in collagen based on atomic force microscope images of the samples. Simulations confirmed the 'speckled' nature of the obtained diffraction patterns. Once inverted, the patterns will show the disposition and orientation of the fibers within the tissue, by enhancing the phase contrast between protein and no protein regions of the sample. Our work affords the application of the most innovative coherent X-ray diffraction tools to the study of biological specimens, and this approach will have a significant impact in biology and medicine because it overcomes many of the limits of current microscopy techniques.

Neutron Diffraction and Electrical Transport Studies on Magnetic Transition in Terbium at High Pressures and Low Temperatures

NASA Astrophysics Data System (ADS)

Thomas, Sarah; Montgomery, Jeffrey; Tsoi, Georgiy; Vohra, Yogesh; Weir, Samuel; Tulk, Christopher; Moreira Dos Santos, Antonio

2013-06-01

Neutron diffraction and electrical transport measurements have been carried out on the heavy rare earth metal terbium at high pressures and low temperatures in order to elucidate its transition from a helical antiferromagnetic to a ferromagnetic ordered phase as a function of pressure. The electrical resistance measurements using designer diamonds show a change in slope as the temperature is lowered through the ferromagnetic Curie temperature. The temperature of the ferromagnetic transition decreases at a rate of -16.7 K/GPa till 3.6 GPa, where terbium undergoes a structural transition from hexagonal close packed (hcp) to an α-Sm phase. Above this pressure, the electrical resistance measurements no longer exhibit a change in slope. In order to confirm the change in magnetic phase suggested by the electrical resistance measurements, neutron diffraction measurements were conducted at the SNAP beamline at the Oak Ridge National Laboratory. Measurements were made at pressures to 5.3 GPa and temperatures as low as 90 K. An abrupt increase in peak intensity in the neutron diffraction spectra signaled the onset of magnetic order below the Curie temperature. A magnetic phase diagram of rare earth metal terbium will be presented to 5.3 GPa and 90 K based on these studies.

High-pressure synthesis of predicted oxynitride perovskite: Yttrium Silicon Oxynitride (YSiO2N)

NASA Astrophysics Data System (ADS)

Ahart, Muhtar; Somayazulu, M.; Vadapoo, Rajasekarakumar; Cohen, R. E.

We synthesized the previously predicted polar oxynitride perovskite in a diamond anvil cell with laser heating. YSiO2N was predicted to have the polar P4mm structure with an effective spontaneous polarization of 130 μC/cm2. A mixture of Yttrium nitride (YN) and amorphous Silicon dioxide (SiO2) were loaded into a diamond anvil cell and laser heated at or above 1200 C at 12 GPa. The run products were investigated by x-ray diffraction, Raman spectroscopy, and second harmonic generation, for their phase and structural properties. The x-ray diffraction pattern (a = 3.235 Å, c = 4.485 Å) shows the phase formation of YSiO2N and matches with the diffraction pattern derived from the first-principle predicted lattice parameters. However, minor unknown peaks are on the diffraction pattern indicating of the co-existence of other unknown phases. Further study of Raman spectroscopy observes the theoretically predicted modes, and second harmonic generation shows strong non-linear optical signal, which confirms the polar properties of YSiO2N. This work is supported by ONR Grants N00014-12-1-1038 and N00014-14-1-0561, by the ERC Advanced Grant ToMCaT.

Synthesis, characterization and bioactivity of a calcium-phosphate glass-ceramics obtained by the sol-gel processing method.

PubMed

Jmal, Nouha; Bouaziz, Jamel

2017-02-01

In this work, a calcium-phosphate glass-ceramics was successfully obtained by heat treatment of a mixture of 26.52 in wt.% of fluorapatite (Fap) and 73.48 in wt.% of 77S (77 SiO 2 14 CaO9 P 2 O 5 in wt.%) gel. The calcium phosphate-glass-ceramics was prepared by sol-gel process with tetraethyl orthosilicate (TEOS), triethyl phosphate (TEP), calcium nitrate and fluorapatite. The synthesized powders were characterized by some commonly used tools such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), 31 P magic angle spinning nuclear magnetic resonance (MAS-NMR), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and thin-film X-ray diffraction (TF-XRD). The obtained results seemed to confirm the nucleation and growth of hydroxyapatite (Hap) nano-phase in the glass. Moreover, an in-vitro evaluation of the glass-ceramic was performed. In addition, to assess its bioactive capacity, it was soaked in simulated body fluid (SBF) at different time intervals. The SEM, EDS and TF-XRD analyses showed the deposition of hydroxyapatite on the surface of the specimens after three days of immersion in SBF solution. The mechanical properties of the obtained material such as rupture strength, Vickers hardness and elastic modulus were measured. In addition, the friction coefficient of calcium phosphate-glass-ceramics was tested. The values of the composite of rupture strength (24MPa), Vickers hardness (214Hv), Young's modulus (52.3GPa), shear modulus (19GPa) and friction coefficient (0.327) were obtained. This glass-ceramics can have useful applications in dental prostheses. Indeed, this material may have promising applications for implants because of its content of fluorine, the effective protector against dental caries. Copyright © 2016 Elsevier B.V. All rights reserved.

Effect of autoclave induced low-temperature degradation on the adhesion energy between yttria-stabilized zirconia veneered with porcelain.

PubMed

Li, Kai Chun; Waddell, J Neil; Prior, David J; Ting, Stephanie; Girvan, Liz; van Vuuren, Ludwig Jansen; Swain, Michael V

2013-11-01

To investigate the effect of autoclave induced low-temperature degradation on the adhesion energy between yttria-stabilized zirconia veneered with porcelain. The strain energy release rate using a four-point bending stable fracture test was evaluated for two different porcelains [leucite containing (VM9) and glass (Zirox) porcelain] veneered to zirconia. Prior to veneering the zirconia had been subjected to 0 (control), 1, 5, 10 and 20 autoclave cycles. The specimens were manufactured to a total bi-layer dimension of 30 mm × 8 mm × 3 mm. Subsequent scanning electron microscopy/energy dispersive spectrometry, electron backscatter diffraction and X-ray diffraction analysis were performed to identify the phase transformation and fracture behavior. The strain energy release rate for debonding of the VM9 specimens were significantly higher (p<0.05) compared to the Zirox specimens across all test groups. Increasing autoclave cycles lowered the strain energy release rate significantly (p<0.05) from 18.67 J/m(2) (control) to the lowest of 12.79 J/m(2) (cycle 10) for only the VM9 specimens. SEM analyses showed predominant cohesive fracture within the porcelain for all cycle groups. XRD analysis of the substrate prior to veneering confirmed a tetragonal to monoclinic phase transformation with increasing the number of autoclave cycles between 5 and 20. The monoclinic phase reverted back to tetragonal phase after undergoing conventional porcelain firing cycles. EBSD data showed significant changes of the grain size distribution between the control and autoclaved specimen (cycle 20). Increasing autoclave cycles only significantly decreased the adhesion of the VM9 layered specimens. In addition, a conventional porcelain firing schedule completely reverted the monoclinic phase back to tetragonal. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Sustained release of anticancer agent phytic acid from its chitosan-coated magnetic nanoparticles for drug-delivery system.

PubMed

Barahuie, Farahnaz; Dorniani, Dena; Saifullah, Bullo; Gothai, Sivapragasam; Hussein, Mohd Zobir; Pandurangan, Ashok Kumar; Arulselvan, Palanisamy; Norhaizan, Mohd Esa

2017-01-01

Chitosan (CS) iron oxide magnetic nanoparticles (MNPs) were coated with phytic acid (PTA) to form phytic acid-chitosan-iron oxide nanocomposite (PTA-CS-MNP). The obtained nanocomposite and nanocarrier were characterized by powder X-ray diffraction, Fourier transform infrared spectroscopy, vibrating sample magnetometry, transmission electron microscopy, and thermogravimetric and differential thermogravimetric analyses. Fourier transform infrared spectra and thermal analysis of MNPs and PTA-CS-MNP nanocomposite confirmed the binding of CS on the surface of MNPs and the loading of PTA in the PTA-CS-MNP nanocomposite. The coating process enhanced the thermal stability of the anticancer nanocomposite obtained. X-ray diffraction results showed that the MNPs and PTA-CS-MNP nanocomposite are pure magnetite. Drug loading was estimated using ultraviolet-visible spectroscopy and showing a 12.9% in the designed nanocomposite. Magnetization curves demonstrated that the synthesized MNPs and nanocomposite were superparamagnetic with saturation magnetizations of 53.25 emu/g and 42.15 emu/g, respectively. The release study showed that around 86% and 93% of PTA from PTA-CS-MNP nanocomposite could be released within 127 and 56 hours by a phosphate buffer solution at pH 7.4 and 4.8, respectively, in a sustained manner and governed by pseudo-second order kinetic model. The cytotoxicity of the compounds on HT-29 colon cancer cells was evaluated by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay. The HT-29 cell line was more sensitive against PTA-CS-MNP nanocomposite than PTA alone. No cytotoxic effect was observed on normal cells (3T3 fibroblast cells). This result indicates that PTA-CS-MNP nanocomposite can inhibit the proliferation of colon cancer cells without causing any harm to normal cell.

Syntheses, crystal structures, and characterization of two new Tl+-Cu2+-Te6+ oxides: Tl4CuTeO6 and Tl6CuTe2O10

NASA Astrophysics Data System (ADS)

Yeon, Jeongho; Kim, Sang-Hwan; Green, Mark A.; Bhatti, Kanwal Preet; Leighton, C.; Shiv Halasyamani, P.

2012-12-01

Crystals and polycrystalline powders of two new oxide materials, Tl4CuTeO6 and Tl6CuTe2O10, have been synthesized by hydrothermal and solid-state methods. The materials were structurally characterized by single-crystal X-ray diffraction. Tl4CuTeO6 and Tl6CuTe2O10 exhibit one dimensional anionic slabs of [CuTeO6]4- and [CuTe2O10]6-, respectively. Common to both slabs is the occurrence of Cu2+O4 distorted squares and Te6+O6 octahedra. The slabs are separated by Tl+ cations. For Tl4CuTeO6, magnetic measurements indicate a maximum at ∼8 K in the temperature dependence of the susceptibility. Low temperature neutron diffraction data confirm no long-range magnetic ordering occurs and the susceptibility was adequately accounted for by fits to a Heisenberg alternating chain model. For Tl6CuTe2O10 on the other hand, magnetic measurements revealed paramagnetism with no evidence of long-range magnetic ordering. Infrared, UV-vis spectra, thermogravimetric, and differential thermal analyses are also reported. Crystal data: Tl4CuTeO6, Triclinic, space group P-1 (No. 2), a=5.8629(8) Å, b=8.7848(11) Å, c=9.2572(12) Å, α=66.0460(10), β=74.2010(10), γ=79.254(2), V=417.70(9) Å3, and Z=2; Tl6CuTe2O10, orthorhombic, space group Pnma (No. 62), a=10.8628(6) Å, b=11.4962(7) Å, c=10.7238(6) Å, V=1339.20(13) Å3, and Z=4.

Modified Bridgman-Stockbarger growth and characterization of LiInSe{sub 2} single crystal

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

Vijayakumar, P., E-mail: ramasamyp@ssn.edu.in; Magesh, M., E-mail: ramasamyp@ssn.edu.in; Arunkumar, A., E-mail: ramasamyp@ssn.edu.in

2014-04-24

The LiInSe{sub 2} polycrystalline materials were successfully synthesized from melt and temperature oscillation method. 8 mm diameter and 32 mm length single crystal was grown from Bridgman-Stockbarger method with steady ampoule rotation. Crystalline phase was confirmed by powder XRD pattern. Thermo gravimetric and differential thermal analysis confirms that the melting point of the grown crystal is 897°C. Rutherford backscattering analysis (RBS) gives the crystal composition as Li{sub 0.8}In{sub 1.16}Se{sub 2.04}. The crystalline perfection of the grown crystal was analyzed by High resolution X-ray diffraction measurements (HRXRD). The electrical properties of the grown crystal were analyzed by Hall effect measurements andmore » it confirms the n-type semiconducting nature.« less

X-ray diffraction and TGA kinetic analyses for chemical looping combustion applications.

PubMed

Tijani, Mansour Mohammedramadan; Aqsha, Aqsha; Mahinpey, Nader

2018-04-01

Synthesis and characterization of supported metal-based oxygen carriers were carried out to provide information related to the use of oxygen carriers for chemical looping combustion processes. The Cu, Co, Fe, Ni metals supported with Al 2 O 3 , CeO 2 , TiO 2 , ZrO 2 were prepared using the wetness impregnation technique. Then, the X-ray Diffraction (XRD) characterization of oxidized and reduced samples was obtained and presented. The kinetic analysis using Thermogravimetric analyzer (TGA) of the synthesized samples was conducted. The kinetics of reduction reaction of all samples were estimated and explained.

Solid-phase data from cores at the proposed Dewey Burdock uranium in-situ recovery mine, near Edgemont, South Dakota

USGS Publications Warehouse

Johnson, Raymond H.; Diehl, Sharon F.; Benzel, William M.

2013-01-01

This report releases solid-phase data from cores at the proposed Dewey Burdock uranium in-situ recovery site near Edgemont, South Dakota. These cores were collected by Powertech Uranium Corporation, and material not used for their analyses were given to the U.S. Geological Survey for additional sampling and analyses. These additional analyses included total carbon and sulfur, whole rock acid digestion for major and trace elements, 234U/238U activity ratios, X-ray diffraction, thin sections, scanning electron microscopy analyses, and cathodoluminescence. This report provides the methods and data results from these analyses along with a short summary of observations.

[Does carbonate originate from carbonate-calcium crystal component of the human urinary calculus?].

PubMed

Yuzawa, Masayuki; Nakano, Kazuhiko; Kumamaru, Takatoshi; Nukui, Akinori; Ikeda, Hitoshi; Suzuki, Kazumi; Kobayashi, Minoru; Sugaya, Yasuhiro; Morita, Tatsuo

2008-09-01

It gives important information in selecting the appropriate treatment for urolithiasis to confirm the component of urinary calculus. Presently component analysis of the urinary calculus is generally performed by infrared spectroscopy which is employed by companies providing laboratory testing services in Japan. The infrared spectroscopy determines the molecular components from the absorption spectra in consequence of atomic vibrations. It has the drawback that an accurate crystal structure cannot be analyzed compared with the X-ray diffraction method which analyzes the crystal constituent based on the diffraction of X-rays on crystal lattice. The components of the urinary calculus including carbonate are carbonate apatite and calcium carbonate such as calcite. Although the latter is reported to be very rare component in human urinary calculus, the results by infrared spectroscopy often show that calcium carbonate is included in calculus. The infrared spectroscopy can confirm the existence of carbonate but cannot determine whether carbonate is originated from carbonate apatite or calcium carbonate. Thus, it is not clear whether calcium carbonate is included in human urinary calculus component in Japan. In this study, we examined human urinary calculus including carbonate by use of X-ray structural analysis in order to elucidate the origin of carbonate in human urinary calculus. We examined 17 human calculi which were reported to contain calcium carbonate by infrared spectroscopy performed in the clinical laboratory. Fifteen calculi were obtained from urinary tract, and two were from gall bladder. The stones were analyzed by X-ray powder method after crushed finely. The reports from the clinical laboratory showed that all urinary culculi consisted of calcium carbonate and calcium phosphate, while the gallstones consisted of calcium carbonate. But the components of all urinary calculi were revealed to be carbonate apatite by X-ray diffraction. The components of gallstones were shown to be calcium carbonate (one calcite and the other aragonite) not only by infrared spectroscopy but by X-ray diffraction. It was shown that component analysis of the calculus could be more accurately performed by adding X-ray diffraction method to infrared spectroscopy. It was shown that calcium carbonate existed in a gallstone. As for the carbonate in human urinary calculi, present study showed that it was not calcium carbonate origin but carbonate apatite origin.

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

Singh, Paviter; Kaur, Manpreet; Singh, Bikramjeet

Boron-carbon core shell structures have been synthesized by solvo-thermal synthesis route. The synthesized material is highly pure. X-ray diffraction analysis confirms the reduction of reactants in to boron and carbon. Scanning Electron Microscopy (SEM) analysis showed that the shell is uniform with average thickness of 340 nm. Photo luminescence studies showed that the material is blue light emitting with CIE color coordinates: x=0.16085, y=0.07554.

Dispersions of TiS2 nanosheets in organic medium

NASA Astrophysics Data System (ADS)

Manjunatha, S.; Kumar, A. Sunil; Machappa, T.

2018-05-01

Here in this article, we report Li-intercalated titanium disulfide (TiS2) two-dimensional (2D) nanosheets, exfoliated in 1-methyl-2-pyrrolidinone (NMP) forming a quite stable dispersions of pale brownish color. As synthesized TiS2 nanosheets were characterized by transmission electron microscopy (TEM). Selected area electron diffraction (SAED) pattern confirmed the hexagonal lattice structure of the exfoliated nanosheets.

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

PubMed

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

2002-11-29

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

Noble-transition metal nanoparticle breathing in a reactive gas atmosphere.

PubMed

Petkov, Valeri; Shan, Shiyao; Chupas, Peter; Yin, Jun; Yang, Lefu; Luo, Jin; Zhong, Chuan-Jian

2013-08-21

In situ high-energy X-ray diffraction coupled to atomic pair distribution function analysis is used to obtain fundamental insight into the effect of the reactive gas environment on the atomic-scale structure of metallic particles less than 10 nm in size. To substantiate our recent discovery we investigate a wide range of noble-transition metal nanoparticles and confirm that they expand and contract radially when treated in oxidizing (O2) and reducing (H2) atmospheres, respectively. The results are confirmed by supplementary XAFS experiments. Using computer simulations guided by the experimental diffraction data we quantify the effect in terms of both relative lattice strain and absolute atomic displacements. In particular, we show that the effect leads to a small percent of extra surface strain corresponding to several tenths of Ångström displacements of the atoms at the outmost layer of the particles. The effect then gradually decays to zero within 4 atomic layers inside the particles. We also show that, reminiscent of a breathing type structural transformation, the effect is reproducible and reversible. We argue that because of its significance and widespread occurrence the effect should be taken into account in nanoparticle research.

Correlation between structural and transport properties of electron beam irradiated PrMnO3 compounds

NASA Astrophysics Data System (ADS)

Christopher, Benedict; Rao, Ashok; Nagaraja, B. S.; Shyam Prasad, K.; Okram, G. S.; Sanjeev, Ganesh; Petwal, Vikash Chandra; Verma, Vijay Pal; Dwivedi, Jishnu; Poornesh, P.

2018-02-01

The structural, electrical, magnetic, and thermal properties of electron beam (EB) irradiated PrMnO3 manganites were investigated in the present communication. X-ray diffraction data reveals that all samples are single phased with orthorhombic distorted structure (Pbnm). Furthermore, the diffracted data are analyzed in detail using Rietveld refinement technique. It is observed that the EB dosage feebly disturbs the MnO6 octahedra. The electrical resistivity of all the samples exhibits semiconducting behavior. Small polaron hopping model is conveniently employed to investigate the semiconducting nature of the pristine as well as EB irradiated samples. The Seebeck coefficient (S) of the pristine as well as the irradiated samples exhibit large positive values at lower temperatures, signifying holes as the dominant charge carriers. The analysis of Seebeck coefficient data confirms that the small polaron hopping mechanism assists the thermoelectric transport property in the high temperature region. The magnetic measurements confirm the existence of paramagnetic (PM) to ferromagnetic (FM) behavior for the pristine and irradiated samples. In the lower temperature regime, coexistence of FM clusters and AFM matrix is dominating. Thus, the complex magnetic behavior of the compound has been explained in terms of rearrangement of antiferromagnetically coupled ionic moments.

A novel conformation of gel grown biologically active cadmium nicotinate

NASA Astrophysics Data System (ADS)

Nair, Lekshmi P.; Bijini, B. R.; Divya, R.; Nair, Prabitha B.; Eapen, S. M.; Dileep Kumar, B. S.; Nishanth Kumar, S.; Nair, C. M. K.; Deepa, M.; Rajendra Babu, K.

2017-11-01

The elimination of toxic heavy metals by the formation of stable co-ordination compounds with biologically active ligands is applicable in drug designing. A new crystalline complex of cadmium with nicotinic acid is grown at ambient temperature using the single gel diffusion method in which the crystal structure is different from those already reported. Single crystal x-ray diffraction reveals the identity of crystal structure belonging to monoclinic system, P21/c space group with cell dimensions a = 17.220 (2) Å, b = 10.2480 (2) Å, c = 7.229(9) Å, β = 91.829(4)°. Powder x-ray diffraction analysis confirmed the crystallinity of the sample. The unidentate mode of co-ordination between the metal atom and the carboxylate group is supported by the Fourier Transform Infra Red spectral data. Thermal analysis ensures the thermal stability of the complex. Kinetic and thermodynamic parameters are also calculated. The stoichiometry of the complex is confirmed by the elemental analysis. The UV-visible spectral analysis shows the wide transparency window of the complex in the visible region. The band gap of the complex is found to be 3.92 eV. The complex shows excellent antibacterial and antifungal activity.

Poly (N-ethyl aniline)/Ag Nanocomposite as Humidity Sensor

NASA Astrophysics Data System (ADS)

Pande, Nishigandh S.; Jaspal, Dipika; Ambekar, Jalindar

Poly (N-ethyl aniline)/Ag organic-inorganic composite has been synthesized by a single step in situ chemical oxidative polymerization method. The synthesis of Poly (N-ethyl aniline)/Ag nanocomposite has been confirmed by X-ray diffraction (XRD), Ultraviolet-Vis Spectroscopy (UV-visible), Fourier transform infrared analysis (FTIR) and FE-SEM investigations. XRD spectral study exhibited major diffraction in the range 20-80∘ (2θ) and indicated the semicrystalline nature of poly (N-ethyl aniline)/Ag nanocomposite. Characteristic peaks in UV-visible and FTIR spectra of poly (N-ethyl aniline) switched to higher wave numbers in poly (N-ethyl aniline)/Ag nanocomposite. Peaks at 1789cm-1, 1595cm-1, 667cm-1 and 501cm-1 in FTIR spectrum confirmed the formation of poly (N-ethyl aniline)/Ag nanocomposite. FE-SEM photographs reported agglomerated granular particulate nature of poly (N-ethyl aniline)/Ag nanocomposite. Synthesized poly (N-ethyl aniline)/Ag nanocomposite exhibited a high response to humidity, good reproducibility and stability at room temperature. An appreciable response was shown in the presence of 40% humid atmosphere for up to successive four cycles. Composite sensitivity has been found to increase with the increasing concentration of humidity, at room temperature.

Growth, crystalline perfection, spectral and optical characterization of a novel optical material: l-tryptophan p-nitrophenol trisolvate single crystal.

PubMed

Sivakumar, N; Srividya, J; Mohana, J; Anbalagan, G

2015-03-15

l-tryptophan p-nitrophenol trisolvate (LTPN), an organic nonlinear optical material was synthesized using ethanol-water mixed solvent and the crystals were grown by a slow solvent evaporation method. The crystal structure and morphology were studied by single crystal X-ray diffraction analysis. The crystalline perfection of the LTPN crystal was analyzed by high-resolution X-ray diffraction study. The molecular structure of the crystal was confirmed by observing the various characteristic functional groups of the material using vibrational spectroscopy. The cut-off wavelength, optical transmission, refractive index and band gap energy were determined using UV-visible data. The variation of refractive index with wavelength shows the normal behavior. The second harmonic generation of the crystal was confirmed and the efficiency was measured using Kurtz Perry powder method. Single and multiple shot methods were employed to measure surface laser damage of the crystal. The photoluminescence spectral study revealed that the emission may be associated with the radiative recombination of trapped electrons and holes. Microhardness measurements revealed that LTPN belongs to a soft material category. Copyright © 2014 Elsevier B.V. All rights reserved.

Microwave synthesis and electrochemical characterization of Mn/Ni mixed oxide for supercapacitor application

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

Prasankumar, T.; Jose, Sujin P., E-mail: sujamystica@yahoo.com; Ilangovan, R.

Nanostructured Mn/Ni mixed metal oxide was synthesized at ambient temperature by facile microwave irradiation technique. The crystal structure and surface morphology were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. X-ray diffraction analysis confirmed the formation of Mn/Ni mixed oxide in rhombohedral phase and the grain size calculated was found to be 87 nm. The irregular spherical morphology of the prepared sample was exhibited by the SEM images. The characteristic peaks of FTIR at about 630 cm{sup −1} and 749 cm{sup −1} were attributed to the Mn-O and Ni-O stretching vibrations respectively. The presence of both Mn and Ni inmore » the prepared sample was validated by the EDS spectra which in turn confirmed the formation of mixed oxide. Cyclic voltammetry and galvanostatic chargedischarge measurements were employed to investigate the electrochemical performance of the mixed oxide. The cyclic voltammetry curves demonstrated good capacitive performance of the sample in the potential window −0.2V to 0.9V. The charge discharge study revealed the suitability of the prepared mixed oxide for the fabrication of supercapacitor electrode.« less

The effect of chemical modification on the physico-chemical characteristics of halloysite: FTIR, XRF, and XRD studies

NASA Astrophysics Data System (ADS)

Szczepanik, Beata; Słomkiewicz, Piotr; Garnuszek, Magdalena; Czech, Kamil; Banaś, Dariusz; Kubala-Kukuś, Aldona; Stabrawa, Ilona

2015-03-01

The effect of chemical modification of halloysite from a Polish strip mine "Dunino" on the chemical composition and structure of this clay mineral was studied using infrared spectroscopy (ATR FT-IR), wavelength dispersive X-ray fluorescence (WDXRF), and X-ray powder diffraction (XRPD) methods. The results obtained by the WDXRF technique confirm that the content of silica and alumina was the highest for bleached halloysite samples and the lowest for acid-treated halloysite. A higher content of Fe2O3 in comparison to halloysite samples coming from other countries was observed for raw halloysite samples. XRPD diffraction pattern obtained for raw halloysite confirmed the presence of halloysite, kaolinite, hematite, and calcite minerals in the sample. Bleaching the halloysite removes (or significantly reduces) the content of other minerals present in the raw halloysite. The FT-IR spectra of the studied halloysite samples show in the 3700-3600 cm-1 region well-defined hydroxyl stretching bands characteristic for the kaolin-group minerals and bands associated with the vibrations of the aluminium-silicon skeleton in the 1400-1000 cm-1 region. Modifying halloysite with 4-chloro-aniline causes successive incorporation of amine into the BH sample.

Rare earth substitution on structural and optical behaviour of CdSe thin films

NASA Astrophysics Data System (ADS)

Singh, Sarika; Shrivastava, A. K.; Tapdiya, Swati

2018-05-01

A series of Sm2+,Gd2+ doped with Cadmium selenide CdSe (x =0.01) has been prepared by using Chemical bath deposition technique. Structural, Optical and Morphological studies were performed using X-ray diffraction (XRD), UV-Visible spectrometer, Raman Studies and Scanning Electron Microscopy (SEM). XRD patterns confirm the samples with Sm,Gd ions, some diffraction peaks appeared which belongs to the cubic phase structure. The values of lattice parameter (a) decreased and particle size decrease on doping. Morphology of the grown films reveals that surface are homogeneous and uniformly spread on the substrates. The elemental analysis of CdSe doped Sm and Gd (1%) different composition was analyzed by Energy Dispersive X-Rays (EDX). The optical values of some important parameters of the studied films were calculated by UVstudy are determined from transmission spectra at wavelength 200 to 900nm. Optical band gap Eg was calculated by tauc relation. Energy band gap of CdSe doped with Sm and Gd varies at 1.8eV and 1.9eV respectively. Bandgap In Raman analysis, a prominent peak shows that confirmation of nano crystalline phase. And intensity of peaks was decreasing after doping.

Phase diagram and electrical behavior of silicon-rich iridium silicide compounds

NASA Technical Reports Server (NTRS)

Allevato, C. E.; Vining, Cronin B.

1992-01-01

The iridium-silicon phase diagram on the silicon-rich side was investigated by means of X-ray powder diffraction, density, differential thermal analysis, metalography, microprobe analysis, and electrical resistivity. Attempts were made to prepare eight previously reported silicon-rich iridium silicide compounds by arc melting and Bridgman-like growth. However, microprobe analysis identified only four distinct compositions: IrSi, Ir3Si4, Ir3Si5 and IrSi sub about 3. The existence of Ir4Si5 could not be confirmed in this study, even though the crystal structure has been previously reported. Differential thermal analysis (DTA) in conjunction with X-ray powder diffraction confirm polymorphism in IrSi sub about 3, determined to have orthorhombic and monoclinic unit cells in the high and low temperature forms. A eutectic composition alloy of 83 +/- 1 atomic percent silicon was observed between IrSi sub about 3 and silicon. Ir3Si4 exhibits distinct metallic behavior while Ir3Si5 is semiconducting. Both and IrSi and IrSi sub about 3 exhibit nearly temperature independent electrical resistivities on the order of 5-10 x 10 exp -6 ohms-m.

Investigation on synthesis, growth and characterization of CdIn2S2Se2 single crystal grown by vertical Bridgman method

NASA Astrophysics Data System (ADS)

Vijayakumar, P.; Ramasamy, P.

2017-06-01

CdIn2S2Se2 polycrystalline material has been synthesized by melt oscillation method. Vertical Bridgman method was used to grow a good quality CdIn2S2Se2 single crystal. The crystalline phase and growth orientation were confirmed by powder X-ray diffraction pattern and unit cell parameters were determined by single crystal X-ray diffraction analysis. The structural uniformity of CdIn2S2Se2 was studied using Raman scattering spectroscopy at room temperature. The stoichiometric composition variation along the CdIn2S2Se2 was measured using energy dispersive spectrometry. The transmission spectra of CdIn2S2Se2 single crystal gave 42% transmission in the NIR region. Thermal property of CdIn2S2Se2 has been studied using differential thermal analysis. Thermal diffusivity, specific heat capacity and thermal conductivity were also measured. Electrical property was measured using Hall Effect measurement and it confirms the n-type semiconducting nature. The hardness behavior has been measured using Vickers micro hardness measurement and the indentation size effect has been observed.

Characterization of the carbides and the martensite phase in powder-metallurgy high-speed steel

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

Godec, Matjaz, E-mail: matjaz.godec@imt.si; Batic, Barbara Setina; Mandrino, Djordje

2010-04-15

A microstructural characterization of the powder-metallurgy high-speed-steel S390 Microclean was performed based on an elemental distribution of the carbide phase as well as crystallographic analyses. The results showed that there were two types of carbides present: vanadium-rich carbides, which were not chemically homogeneous and exhibited a tungsten-enriched or tungsten-depleted central area; and chemically homogeneous tungsten-rich M{sub 6}C-type carbides. Despite the possibility of chemical inhomogenities, the crystallographic orientation of each of the carbides was shown to be uniform. Using electron backscatter diffraction the vanadium-rich carbides were determined to be either cubic VC or hexagonal V{sub 6}C{sub 5}, while the tungsten-rich carbidesmore » were M{sub 6}C. The electron backscatter diffraction results were also verified using X-ray diffraction. Several electron backscatter diffraction pattern maps were acquired in order to define the fraction of each carbide phase as well as the amount of martensite phase. The fraction of martensite was estimated using band-contrast images, while the fraction of carbides was calculated using the crystallographic data.« less

Thermal phase transition behavior of lipid layers on a single human corneocyte cell.

PubMed

Imai, Tomohiro; Nakazawa, Hiromitsu; Kato, Satoru

2013-09-01

We have improved the selected area electron diffraction method to analyze the dynamic structural change in a single corneocyte cell non-invasively stripped off from human skin surface. The improved method made it possible to obtain reliable diffraction images to trace the structural change in the intercellular lipid layers on a single corneocyte cell during heating from 24°C to 100°C. Comparison of the results with those of synchrotron X-ray diffraction experiments on human stratum corneum sheets revealed that the intercellular lipid layers on a corneocyte cell exhibit essentially the same thermal phase transitions as those in a stratum corneum sheet. These results suggest that the structural features of the lipid layers are well preserved after the mechanical stripping of the corneocyte cell. Moreover, electron diffraction analyses of the thermal phase transition behaviors of the corneocyte cells that had the lipid layers with different distributions of orthorhombic and hexagonal domains at 24°C suggested that small orthorhombic domains interconnected with surrounding hexagonal domains transforms in a continuous manner into new hexagonal domains. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Radiometric assessment method for diffraction effects in hyperspectral imagers applied to the earth explorer #8 mission candidate flex

NASA Astrophysics Data System (ADS)

Berlich, R.; Harnisch, B.

2017-11-01

An accurate stray light analysis represents a crucial part in the early design phase of hyperspectral imaging systems, since scattering effects can severely limit the radiometric accuracy performance. In addition to conventional contributors including ghost images and surface scattering, i.e. caused by a residual surface micro-roughness and particle contamination, diffraction effects can result in significant radiometric errors in the spatial and spectral domain of pushbroom scanners. In this paper, we present a mathematical approach that efficiently evaluates these diffraction effects based on a Fourier analysis. It is shown that considering the conventional diffraction at the systems entrance pupil only, significantly overestimates the stray light contribution. In fact, a correct assessment necessitates taking into account the joint influence of the entrance pupil, the spectrometer slit as well as the dispersion element. We quantitatively investigate the corresponding impact on the Instrument Spectral Response Function (ISRF) of the Earth Explorer #8 Mission Candidate FLEX and analyse the expected radiometric error distribution for a typical earth observation scenario requirement.

Detecting Negative Obstacles by Use of Radar

NASA Technical Reports Server (NTRS)

Mittskus, Anthony; Lux, James

2006-01-01

Robotic land vehicles would be equipped with small radar systems to detect negative obstacles, according to a proposal. The term "negative obstacles" denotes holes, ditches, and any other terrain features characterized by abrupt steep downslopes that could be hazardous for vehicles. Video cameras and other optically based obstacle-avoidance sensors now installed on some robotic vehicles cannot detect obstacles under adverse lighting conditions. Even under favorable lighting conditions, they cannot detect negative obstacles. A radar system according to the proposal would be of the frequency-modulation/ continuous-wave (FM/CW) type. It would be installed on a vehicle, facing forward, possibly with a downward slant of the main lobe(s) of the radar beam(s) (see figure). It would utilize one or more wavelength(s) of the order of centimeters. Because such wavelengths are comparable to the characteristic dimensions of terrain features associated with negative hazards, a significant amount of diffraction would occur at such features. In effect, the diffraction would afford a limited ability to see corners and to see around corners. Hence, the system might utilize diffraction to detect corners associated with negative obstacles. At the time of reporting the information for this article, preliminary analyses of diffraction at simple negative obstacles had been performed, but an explicit description of how the system would utilize diffraction was not available.

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

McCormac, Kathleen; Byrd, Ian; Brannen, Rodney

We prepared highly porous Si/TiO 2 composite nanofibres using a unique sulphur-templating method combined with electrospinning. The structure, morphology, surface area, phase and composition of these nanofibres were characterized using Raman spectroscopy, scanning electron microscopy, powder X-ray diffraction, surface area analyser and thermogravimetric analyser. The specific surface area of Si/TiO 2 porous NFs is as large as 387m 2g -1, whose silicon capacity can be maintained above 1580mAhg -1 in 180 cycles.

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

Bourlier, Yoan; Cristini Robbe, Odile; Laboratoire de Physique des Lasers, Atomes et Molécules

Highlights: • CuIn{sub (1−x)}Ga{sub x}S{sub 2} thin films were prepared by sol–gel process. • Evolution of lattice parameters is characteristic of a solid solution. • Optical band gap was found to be linearly dependent on the gallium rate. - Abstract: In this paper, we report the elaboration of Cu(In,Ga)S{sub 2} chalcopyrite thin films via a sol–gel process. To reach this aim, solutions containing copper, indium and gallium complexes were prepared. These solutions were thereafter spin-coated onto the soda lime glass substrates and calcined, leading to metallic oxides thin films. Expected chalcopyrite films were finally obtained by sulfurization of oxides layersmore » using a sulfur atmosphere at 500 °C. The rate of gallium incorporation was studied both at the solutions synthesis step and at the thin films sulfurization process. Elemental and X-ray diffraction (XRD) analyses have shown the efficiency of monoethanolamine used as a complexing agent for the preparation of CuIn{sub (1−x)}Ga{sub x}S{sub 2} thin layers. Moreover, the replacement of diethanolamine by monoethanolamine has permitted the substitution of indium by isovalent gallium from x = 0 to x = 0.4 and prevented the precipitation of copper derivatives. XRD analyses of sulfurized thin films CuIn{sub (1−x)}Ga{sub x}S{sub 2,} clearly indicated that the increasing rate of gallium induced a shift of XRD peaks, revealing an evolution of the lattice parameter in the chalcopyrite structure. These results were confirmed by Raman analyses. Moreover, the optical band gap was also found to be linearly dependent upon the gallium rate incorporated within the thin films: it varies from 1.47 eV for x = 0 to 1.63 eV for x = 0.4.« less

3-D microstructure of olivine in complex geological materials reconstructed by correlative X-ray μ-CT and EBSD analyses.

PubMed

Kahl, W-A; Dilissen, N; Hidas, K; Garrido, C J; López-Sánchez-Vizcaíno, V; Román-Alpiste, M J

2017-11-01

We reconstruct the 3-D microstructure of centimetre-sized olivine crystals in rocks from the Almirez ultramafic massif (SE Spain) using combined X-ray micro computed tomography (μ-CT) and electron backscatter diffraction (EBSD). The semidestructive sample treatment involves geographically oriented drill pressing of rocks and preparation of oriented thin sections for EBSD from the μ-CT scanned cores. The μ-CT results show that the mean intercept length (MIL) analyses provide reliable information on the shape preferred orientation (SPO) of texturally different olivine groups. We show that statistical interpretation of crystal preferred orientation (CPO) and SPO of olivine becomes feasible because the highest densities of the distribution of main olivine crystal axes from EBSD are aligned with the three axes of the 3-D ellipsoid calculated from the MIL analyses from μ-CT. From EBSD data we distinguish multiple CPO groups and by locating the thin sections within the μ-CT volume, we assign SPO to the corresponding olivine crystal aggregates, which confirm the results of statistical comparison. We demonstrate that the limitations of both methods (i.e. no crystal orientation data in μ-CT and no spatial information in EBSD) can be overcome, and the 3-D orientation of the crystallographic axes of olivines from different orientation groups can be successfully correlated with the crystal shapes of representative olivine grains. Through this approach one can establish the link among geological structures, macrostructure, fabric and 3-D SPO-CPO relationship at the hand specimen scale even in complex, coarse-grained geomaterials. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Relation between textured surface and diffuse reflectance of Cu films

NASA Astrophysics Data System (ADS)

Shukla, Gaurav; Angappane, S.

2018-04-01

Cu nanostructures namely chevron, slanted and vertical posts deposited on Si substrate by glancing angle deposition (GLAD) technique using DC magnetron sputtering are studied to understand the optical reflectance properties of various textures. The X-ray diffraction analysis confirmed the crystalline nature of the different structures of deposited Cu films. The FESEM images confirmed the formation of chevron, slanted and vertical posts. From the optical reflectance spectra, we found that the reflectance is more for chevron than vertical and slanted posts which have almost the same reflectance over the entire wavelength. The films with chevron texture would find various applications, like, light detector, light trapping, sensors etc.

Tailoring growth conditions for efficient tuning of band edge of CdS nanoparticles

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

Susha, N.; Nair, Swapna S., E-mail: swapna.s.nair@gmail.com; Aravind, P. B.

2015-06-24

CdS nanoparticles are successively synthesized by chemical precipitation method. The samples prepared at different reaction time and temperature are characterized by X-ray diffraction, Diffuse reflectance spectroscopy, Photoluminescence spectroscopy ans Energy dispersive x-ray analysis. Visible color variation is noted from light yellow to orange, indicates the quantum confinement effect and the results are again got confirmed from the optical studies. A shift in absorption peak is observed towards the lower region of the visible spectra - the “blue shift”- upon decrease in reaction time and temperature. Blue emission observed in the photoluminescence spectrum confirms the grain size induced confinement.

Structural and dielectric studies of Ce doped BaSnO3 perovskite nanostructures

NASA Astrophysics Data System (ADS)

Angel, S. Lilly; Deepa, K.; Rajamanickam, N.; Jayakumar, K.; Ramachandran, K.

2018-04-01

Undoped and Cerium (Ce) doped BaSnO3(BSO) nanostructures were synthesized by co-precipitation method. The cubic structure and perovskite phase were confirmed by X-ray diffraction (XRD). The crystallite size of BSO is 41nm and when Ce ion concentration is increased, the crystallite sizesdecreased. The nanocube, nanocuboids and nanorods are observed from SEM analysis. The purity of the undoped and doped samples are confirmed by EDS spectrum. For larger defects, wide band gap was obtained from UV-Vis and PL spectrum. The dielectric constants are increased at low frequencies when Ce impurities are introduced in the BSO matrix at Sn site.

Crystallography of refractory metal nuggets in carbonaceous chondrites: A transmission Kikuchi diffraction approach

NASA Astrophysics Data System (ADS)

Daly, Luke; Bland, Phil A.; Dyl, Kathryn A.; Forman, Lucy V.; Saxey, David W.; Reddy, Steven M.; Fougerouse, Denis; Rickard, William D. A.; Trimby, Patrick W.; Moody, Steve; Yang, Limei; Liu, Hongwei; Ringer, Simon P.; Saunders, Martin; Piazolo, Sandra

2017-11-01

Transmission Kikuchi diffraction (TKD) is a relatively new technique that is currently being developed for geological sample analysis. This technique utilises the transmission capabilities of a scanning electron microscope (SEM) to rapidly and accurately map the crystallographic and geochemical features of an electron transparent sample. TKD uses a similar methodology to traditional electron backscatter diffraction (EBSD), but is capable of achieving a much higher spatial resolution (5-10 nm) (Trimby, 2012; Trimby et al., 2014). Here we apply TKD to refractory metal nuggets (RMNs) which are micrometre to sub-micrometre metal alloys composed of highly siderophile elements (HSEs) found in primitive carbonaceous chondrite meteorites. TKD allows us to analyse RMNs in situ, enabling the characterisation of nanometre-scale variations in chemistry and crystallography, whilst preserving their spatial and crystallographic context. This provides a complete representation of each RMN, permitting detailed interpretation of their formation history. We present TKD analysis of five transmission electron microscopy (TEM) lamellae containing RMNs coupled with EBSD and TEM analyses. These analyses revealed textures and relationships not previously observed in RMNs. These textures indicate some RMNs experienced annealing, forming twins. Some RMNs also acted as nucleation centres, and formed immiscible metal-silicate fluids. In fact, each RMN analysed in this study had different crystallographic textures. These RMNs also had heterogeneous compositions, even between RMNs contained within the same inclusion, host phase and even separated by only a few nanometres. Some RMNs are also affected by secondary processes at low temperature causing exsolution of molybdenite. However, most RMNs had crystallographic textures indicating that the RMN formed prior to their host inclusion. TKD analyses reveal most RMNs have been affected by processing in the protoplanetary disk. Despite this alteration, RMNs still preserve primary crystallographic textures and heterogeneous chemical signatures. This heterogeneity in crystallographic relationships, which mostly suggest that RMNs pre-date their host, is consistent with the idea that there is not a dominant RMN forming process. Each RMN has experienced a complex history, supporting the suggestion of Daly et al. (2017), that RMNs may preserve a diverse pre-solar chemical signature inherited from the Giant Molecular Cloud.

An In-situ method for the study of strain broadening usingsynchrotronx-ray diffraction

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

Tang, Chiu C.; Lynch, Peter A.; Cheary, Robert W.

2006-12-15

A tensonometer for stretching metal foils has beenconstructed for the study of strain broadening in x-ray diffraction lineprofiles. This device, which is designed for use on the powderdiffractometer in Station 2.3 at Daresbury Laboratory, allows in-situmeasurements to be performed on samples under stress. It can be used fordata collection in either transmission or reflection modes using eithersymmetric or asymmetric diffraction geometries. As a test case,measurements were carried out on a 18mum thick copper foil experiencingstrain levels of up to 5 percent using both symmetric reflection andsymmetric transmission diffraction. All the diffraction profilesdisplayed peak broadening and asymmetry which increased with strain.more » Themeasured profiles were analysed by the fundamental parameters approachusing the TOPAS peak fitting software. All the observed broadenedprofiles were modelled by convoluting a refineable diffraction profile,representing the dislocation and crystallite size broadening, with afixed instrumental profile pre-determined usinghigh quality LaB6reference powder. The de-convolution process yielded "pure" sampleintegral breadths and asymmetry results which displayed a strongdependence on applied strain and increased almost linearly with appliedstrain. Assuming crystallite size broadening in combination withdislocation broadening arising from fcc a/2<110>111 dislocations,we have extracted the variation of mechanic al property with strain. Theobservation of both peak asymmetry and broadening has been interpreted asa manifestation of a cellular structure with cell walls and cellinteriors possessing high and low dislocation densities.« less