Atomically resolved structural determination of graphene and its point defects via extrapolation assisted phase retrieval

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

Latychevskaia, Tatiana; Fink, Hans-Werner

Previously reported crystalline structures obtained by an iterative phase retrieval reconstruction of their diffraction patterns seem to be free from displaying any irregularities or defects in the lattice, which appears to be unrealistic. We demonstrate here that the structure of a nanocrystal including its atomic defects can unambiguously be recovered from its diffraction pattern alone by applying a direct phase retrieval procedure not relying on prior information of the object shape. Individual point defects in the atomic lattice are clearly apparent. Conventional phase retrieval routines assume isotropic scattering. We show that when dealing with electrons, the quantitatively correct transmission functionmore » of the sample cannot be retrieved due to anisotropic, strong forward scattering specific to electrons. We summarize the conditions for this phase retrieval method and show that the diffraction pattern can be extrapolated beyond the original record to even reveal formerly not visible Bragg peaks. Such extrapolated wave field pattern leads to enhanced spatial resolution in the reconstruction.« less

Transparent Glass Ceramics Doped by Chromium(III) and Chromium(III) and Neodymium(III) as New Materials for Lasers and Luminescent Solar Concentrators.

DTIC Science & Technology

1987-04-30

1.5 ZrO2 * 0.3 As203, 0.024 Cr203, melted under various conditions. Parallel measurements of X-ray diffraction, optical and EPR spectra reveal the...optical and EPR spectra reveal the different formation of gahnite from precursor glass or petalite-like phase. Introduction In a number of recent...conditions on optical and EPR spectra of Cr(III). Further on the parallel changes of spectra and x-ray diffraction patterns are indica- ted. The gahnite

Structural and spectroscopic study of mechanically synthesized SnO{sub 2} nanostructures

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

Vij, Ankush, E-mail: vij-anx@yahoo.com; Kumar, Ravi; Presently at Beant College of Engineering and Technology, Gurdaspur-143521

2016-05-23

We report the single step synthesis of SnO{sub 2} nanostructures using high energy mechanical attrition method. X-ray diffraction (XRD) pattern reveals the single phase rutile structure with appreciable broadening of diffraction peaks, which is a signature of nanostructure formation. The average crystallite size of SnO{sub 2} nanostructures has been calculated to be ~15 nm. The micro-Raman study reveals the shifting of A{sub 1g} Raman mode towards lower wave number, which is correlated with the nanostructure formation.

Three-dimensional Bragg diffraction in growth-disordered opals

NASA Astrophysics Data System (ADS)

Baryshev, A. V.; Kaplyanskii, Alexander A.; Kosobukin, Vladimir A.; Limonov, M. F.; Samusev, K. B.; Usvyat, D. E.

2003-06-01

After artificial opals as well as opal-based infilled and inverted composites are considered to be promising representatives of photonic crystal materials. Earlier, photonic stop gaps in opals were studied mainly in transmission or specular reflection geometries corresponding to "one-dimensional" Bragg diffraction. On the contrary, this work was aimed at observing the typical patterns of optical Bragg diffraction in which phenomenon opal crystal structure acts as a three-dimensional diffraction grating. Although our experiments were performed for artificial opals possessing unavoidable imperfections a well-pronounced diffraction peaks were observed characteristic of a crystal structure. Each of the diffraction maxima reveals a photonic stop gap in the specified direction, while the spectral width of the peak is a measure of the photonic stop gap width.

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.

One-Dimensional Scanning Approach to Shock Sensing

NASA Technical Reports Server (NTRS)

Tokars, Roger; Adamovsky, Girgory; Floyd, Bertram

2009-01-01

Measurement tools for high speed air flow are sought both in industry and academia. Particular interest is shown in air flows that exhibit aerodynamic shocks. Shocks are accompanied by sudden changes in density, pressure, and temperature. Optical detection and characterization of such shocks can be difficult because the medium is normally transparent air. A variety of techniques to analyze these flows are available, but they often require large windows and optical components as in the case of Schlieren measurements and/or large operating powers which precludes their use for in-flight monitoring and applications. The one-dimensional scanning approach in this work is a compact low power technique that can be used to non-intrusively detect shocks. The shock is detected by analyzing the optical pattern generated by a small diameter laser beam as it passes through the shock. The optical properties of a shock result in diffraction and spreading of the beam as well as interference fringes. To investigate the feasibility of this technique a shock is simulated by a 426 m diameter optical fiber. Analysis of results revealed a direct correlation between the optical fiber or shock location and the beam s diffraction pattern. A plot of the width of the diffraction pattern vs. optical fiber location reveals that the width of the diffraction pattern was maximized when the laser beam is directed at the center of the optical fiber. This work indicates that the one-dimensional scanning approach may be able to determine the location of an actual shock. Near and far field effects associated with a small diameter laser beam striking an optical fiber used as a simulated shock are investigated allowing a proper one-dimensional scanning beam technique.

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.

Structural investigation of porcine stomach mucin by X-ray fiber diffraction and homology modeling

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

Veluraja, K., E-mail: veluraja@msuniv.ac.in; Vennila, K.N.; Umamakeshvari, K.

Research highlights: {yields} Techniques to get oriented mucin fibre. {yields} X-ray fibre diffraction pattern for mucin. {yields} Molecular modeling of mucin based on X-ray fibre diffraction pattern. -- Abstract: The basic understanding of the three dimensional structure of mucin is essential to understand its physiological function. Technology has been developed to achieve orientated porcine stomach mucin molecules. X-ray fiber diffraction of partially orientated porcine stomach mucin molecules show d-spacing signals at 2.99, 4.06, 4.22, 4.7, 5.37 and 6.5 A. The high intense d-spacing signal at 4.22 A is attributed to the antiparallel {beta}-sheet structure identified in the fraction of themore » homology modeled mucin molecule (amino acid residues 800-980) using Nidogen-Laminin complex structure as a template. The X-ray fiber diffraction signal at 6.5 A reveals partial organization of oligosaccharides in porcine stomach mucin. This partial structure of mucin will be helpful in establishing a three dimensional structure for the whole mucin molecule.« less

PVA/NaCl/MgO nanocomposites-microstructural analysis by whole pattern fitting method

NASA Astrophysics Data System (ADS)

Prashanth, K. S.; Mahesh, S. S.; Prakash, M. B. Nanda; Somashekar, R.; Nagabhushana, B. M.

2018-04-01

The nanofillers in the macromolecular matrix have displayed noteworthy changes in the structure and reactivity of the polymer nanocomposites. Novel functional materials usually consist of defects and are largely disordered. The intriguing properties of these materials are often attributed to defects. X-ray line profiles from powder diffraction reveal the quantitative information about size distribution and shape of diffracting domains which governs the contribution from small conventional X-ray diffraction (XRD) techniques to enumerate the microstructural information. In this study the MgO nanoparticles were prepared by solution combustion method and PVA/NaCl/MgO nanocomposite films were synthesized by the solvent cast method. Microstructural parameters viz crystal defects like stacking faults and twin faults, compositional inhomogeneity, crystallite size and lattice strain (g in %), were extracted using whole pattern fitting method.

Dissociation behavior of methane--ethane mixed gas hydrate coexisting structures I and II.

PubMed

Kida, Masato; Jin, Yusuke; Takahashi, Nobuo; Nagao, Jiro; Narita, Hideo

2010-09-09

Dissociation behavior of methane-ethane mixed gas hydrate coexisting structures I and II at constant temperatures less than 223 K was studied with use of powder X-ray diffraction and solid-state (13)C NMR techniques. The diffraction patterns at temperatures less than 203 K showed both structures I and II simultaneously convert to Ih during the dissociation, but the diffraction pattern at temperatures greater than 208 K showed different dissociation behavior between structures I and II. Although the diffraction peaks from structure II decreased during measurement at constant temperatures greater than 208 K, those from structure I increased at the initial step of dissociation and then disappeared. This anomalous behavior of the methane-ethane mixed gas hydrate coexisting structures I and II was examined by using the (13)C NMR technique. The (13)C NMR spectra revealed that the anomalous behavior results from the formation of ethane-rich structure I. The structure I hydrate formation was associated with the dissociation rate of the initial methane-ethane mixed gas hydrate.

Effect of processing on the microstructure of finger millet by X-ray diffraction and scanning electron microscopy.

PubMed

Dharmaraj, Usha; Parameswara, P; Somashekar, R; Malleshi, Nagappa G

2014-03-01

Finger millet is one of the important minor cereals, and carbohydrates form its major chemical constituent. Recently, the millet is processed to prepare hydrothermally treated (HM), decorticated (DM), expanded (EM) and popped (PM) products. The present research aims to study the changes in the microstructure of carbohydrates using X-ray diffraction and scanning electron microscopy. Processing the millet brought in significant changes in the carbohydrates. The native millet exhibited A-type pattern of X-ray diffraction with major peaks at 2θ values of 15.3, 17.86 and 23.15°, whereas, all other products showed V-type pattern with single major peak at 2θ values ranging from 19.39 to 19.81°. The corresponding lattice spacing and the number of unit cells in a particular direction of reflection also reduced revealing that crystallinity of starch has been decreased depending upon the processing conditions. Scanning electron microscopic studies also revealed that the orderly pattern of starch granules changed into a coherent mass due to hydrothermal treatment, while high temperature short time treatment rendered a honey-comb like structure to the product. However, the total carbohydrates and non-starch polysaccharide contents almost remained the same in all the products except for DM and EM, but the individual carbohydrate components changed significantly depending on the type of processing.

Fourier-Based Diffraction Analysis of Live Caenorhabditis elegans.

PubMed

Magnes, Jenny; Hastings, Harold M; Raley-Susman, Kathleen M; Alivisatos, Clara; Warner, Adam; Hulsey-Vincent, Miranda

2017-09-13

This manuscript describes how to classify nematodes using temporal far-field diffraction signatures. A single C. elegans is suspended in a water column inside an optical cuvette. A 632 nm continuous wave HeNe laser is directed through the cuvette using front surface mirrors. A significant distance of at least 20-30 cm traveled after the light passes through the cuvette ensures a useful far-field (Fraunhofer) diffraction pattern. The diffraction pattern changes in real time as the nematode swims within the laser beam. The photodiode is placed off-center in the diffraction pattern. The voltage signal from the photodiode is observed in real time and recorded using a digital oscilloscope. This process is repeated for 139 wild type and 108 "roller" C. elegans. Wild type worms exhibit a rapid oscillation pattern in solution. The "roller" worms have a mutation in a key component of the cuticle that interferes with smooth locomotion. Time intervals that are not free of saturation and inactivity are discarded. It is practical to divide each average by its maximum to compare relative intensities. The signal for each worm is Fourier transformed so that the frequency pattern for each worm emerges. The signal for each type of worm is averaged. The averaged Fourier spectra for the wild type and the "roller" C. elegans are distinctly different and reveal that the dynamic worm shapes of the two different worm strains can be distinguished using Fourier analysis. The Fourier spectra of each worm strain match an approximate model using two different binary worm shapes that correspond to locomotory moments. The envelope of the averaged frequency distribution for actual and modeled worms confirms the model matches the data. This method can serve as a baseline for Fourier analysis for many microscopic species, as every microorganism will have its unique Fourier spectrum.

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 .

Laser scattering induced holograms in lithium niobate. [observation of diffraction cones

NASA Technical Reports Server (NTRS)

Magnusson, R.; Gaylord, T. K.

1974-01-01

A 3.0-mm thick poled single crystal of lithium niobate doped with 0.1 mole% iron was exposed to a single beam and then to two intersecting beams of an argon ion laser operating at 515-nm wavelength. Laser scattering induced holograms were thus written and analyzed. The presence of diffraction cones was observed and is shown to result from the internally recorded interference pattern resulting from the interference of the original incident laser beam with light scattered from material inhomogeneities. This phenomenon is analyzed using Ewald sphere construction techniques which reveal the geometrical relationships existing for the diffraction cones.

Detection of nanoscale embedded layers using laboratory specular X-ray diffraction

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

Beekman, Matt, E-mail: matt.beekman@oit.edu; Rodriguez, Gabriel; Atkins, Ryan

Unusual specular X-ray diffraction patterns have been observed from certain thin film intergrowths of metal monochalcogenide (MX) and transition metal dichalcogenide (TX{sub 2}) structures. These patterns exhibit selective “splitting” or broadening of selected (00l) diffraction peaks, while other (00l) reflections remain relatively unaffected [Atkins et al., Chem. Mater. 24, 4594 (2012)]. Using a simplified optical model in the kinematic approximation, we illustrate that these peculiar and somewhat counterintuitive diffraction features can be understood in terms of additional layers of one of the intergrowth components, MX or TX{sub 2}, interleaved between otherwise “ideal” regions of MX-TX{sub 2} intergrowth. The interpretation ismore » in agreement with scanning transmission electron microscope imaging, which reveals the presence of such stacking “defects” in films prepared from non-ideal precursors. In principle, the effect can be employed as a simple, non-destructive laboratory probe to detect and characterize ultrathin layers of one material, e.g., 2-dimensional crystals, embedded between two slabs of a second material, effectively using the two slabs as a highly sensitive interferometer of their separation distance.« less

Glass transition in ferroic glass K x (ND4)1-x D2PO4: a complete x-ray diffraction line shape analysis

NASA Astrophysics Data System (ADS)

Ranjan Choudhury, Rajul; Chitra, R.; Jayakrishnan, V. B.

2016-03-01

Quenching of dynamic disorder in glassy systems is termed as the glass transition. Ferroic glasses belong to the class of paracrystalline materials having crystallographic order in-between that of a perfect crystal and amorphous material, a classic example of ferroic glass is the solid solution of ferroelectric deuterated potassium dihydrogen phosphate and antiferroelectric deuterated ammonium dihydrogen phosphate. Lowering temperature of this ferroic glass can lead to a glass transition to a quenched disordered state. The subtle atomic rearrangement that takes place at such a glass transition can be revealed by careful examination of the temperature induced changes occurring in the x-ray powder diffraction (XRD) patterns of these materials. Hence we report here results of a complete diffraction line shape analysis of the XRD patterns recorded at different temperatures from deuterated mixed crystals DK x A1-x DP with mixing concentration x ranging as 0 < x < 1. Changes observed in diffraction peak shapes have been explained on the basis of structural rearrangements induced by changing O-D-O hydrogen bond dynamics in these paracrystals.

Phase retrieval of images using Gaussian radial bases.

PubMed

Trahan, Russell; Hyland, David

2013-12-20

Here, the possibility of a noniterative solution to the phase retrieval problem is explored. A new look is taken at the phase retrieval problem that reveals that knowledge of a diffraction pattern's frequency components is enough to recover the image without projective iterations. This occurs when the image is formed using Gaussian bases that give the convenience of a continuous Fourier transform existing in a compact form where square pixels do not. The Gaussian bases are appropriate when circular apertures are used to detect the diffraction pattern because of their optical transfer functions, as discussed briefly. An algorithm is derived that is capable of recovering an image formed by Gaussian bases from only the Fourier transform's modulus, without background constraints. A practical example is shown.

Studies of cavitation and ice nucleation in 'doubly-metastable' water: time-lapse photography and neutron diffraction.

PubMed

Barrow, Matthew S; Williams, P Rhodri; Chan, Hoi-Houng; Dore, John C; Bellissent-Funel, Marie-Claire

2012-10-14

High-speed photographic studies and neutron diffraction measurements have been made of water under tension in a Berthelot tube. Liquid water was cooled below the normal ice-nucleation temperature and was in a doubly-metastable state prior to a collapse of the liquid state. This transition was accompanied by an exothermic heat release corresponding with the rapid production of a solid phase nucleated by cavitation. Photographic techniques have been used to observe the phase transition over short time scales in which a solidification front is observed to propagate through the sample. Significantly, other images at a shorter time interval reveal the prior formation of cavitation bubbles at the beginning of the process. The ice-nucleation process is explained in terms of a mechanism involving hydrodynamically-induced changes in tension in supercooled water in the near vicinity of an expanding cavitation bubble. Previous explanations have attributed the nucleation of the solid phase to the production of high positive pressures. Corresponding results are presented which show the initial neutron diffraction pattern after ice-nucleation. The observed pattern does not exhibit the usual crystalline pattern of hexagonal ice [I(h)] that is formed under ambient conditions, but indicates the presence of other ice forms. The composite features can be attributed to a mixture of amorphous ice, ice-I(h)/I(c) and the high-pressure form, ice-III, and the diffraction pattern continues to evolve over a time period of about an hour.

Growth, crystalline perfection, spectral, thermal and theoretical studies on imidazolium L-tartrate crystals.

PubMed

Meena, K; Muthu, K; Meenatchi, V; Rajasekar, M; Bhagavannarayana, G; Meenakshisundaram, S P

2014-04-24

Transparent optical quality single crystals of imidazolium L-tartrate (IMLT) were grown by conventional slow evaporation solution growth technique. Crystal structure of the as-grown IMLT was determined by single crystal X-ray diffraction analysis. Thermal analysis reveals the purity of the crystal and the sample is stable up to the melting point. Good transmittance in the visible region is observed and the band gap energy is estimated using diffuse reflectance data by the application of Kubelka-Munk algorithm. The powder X-ray diffraction study reveals the crystallinity of the as-grown crystal and it is compared with that of the experimental one. An additional peak in high resolution X-ray diffraction (HRXRD) indicates the presence of an internal structural low angle boundary. Second harmonic generation (SHG) activity of IMLT is significant as estimated by Kurtz and Perry powder technique. HOMO-LUMO energies and first-order molecular hyperpolarizability of IMLT have been evaluated using density functional theory (DFT) employing B3LYP functional and 6-31G(d,p) basis set. The optimized geometry closely resembles the ORTEP. The vibrational patterns present in the molecule are confirmed by FT-IR coinciding with theoretical patterns. Copyright © 2014 Elsevier B.V. All rights reserved.

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

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.

Crystal structure of human tooth enamel studied by neutron diffraction

NASA Astrophysics Data System (ADS)

Ouladdiaf, Bachir; Rodriguez-Carvajal, Juan; Goutaudier, Christelle; Ouladdiaf, Selma; Grosgogeat, Brigitte; Pradelle, Nelly; Colon, Pierre

2015-02-01

Crystal structure of human tooth enamel was investigated using high-resolution neutron powder diffraction. Excellent agreement between observed and refined patterns is obtained, using the hexagonal hydroxyapatite model for the tooth enamel, where a large hydroxyl deficiency ˜70% is found in the 4e site. Rietveld refinements method combined with the difference Fourier maps have revealed, however, that the hydroxyl ions are not only disordered along the c-axis but also within the basal plane. Additional H ions located at the 6h site and forming HPO42- anions were found.

Characterization of CuCl quantum dots grown in NaCl single crystals via optical measurements, X-ray diffraction, and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Miyajima, Kensuke; Akatsu, Tatsuro; Itoh, Ken

2018-05-01

We evaluated the crystal size, shape, and alignment of the lattice planes of CuCl quantum dots (QDs) embedded in NaCl single crystals by optical measurements, X-ray diffraction (XRD) patterns, and transmission electron microscopy (TEM). We obtained, for the first time, an XRD pattern and TEM images for CuCl QDs in NaCl crystals. The XRD pattern showed that the lattice planes of the CuCl QDs were parallel to those of the NaCl crystals. In addition, the size of the QDs was estimated from the diffraction width. It was apparent from the TEM images that almost all CuCl QDs were polygonal, although some cubic QDs were present. The mean size and size distribution of the QDs were also obtained. The dot size obtained from optical measurements, XRD, and TEM image were almost consistent. Our new findings can help to reveal the growth mechanism of semiconductor QDs embedded in a crystallite matrix. In addition, this work will play an important role in progressing the study of optical phenomena originating from assembled semiconductor QDs.

Determination of the geometric corrugation of graphene on SiC(0001) by grazing incidence fast atom diffraction

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

Zugarramurdi, A.; Debiossac, M.; Lunca-Popa, P.

2015-03-09

We present a grazing incidence fast atom diffraction (GIFAD) study of monolayer graphene on 6H-SiC(0001). This system shows a Moiré-like 13 × 13 superlattice above the reconstructed carbon buffer layer. The averaging property of GIFAD results in electronic and geometric corrugations that are well decoupled; the graphene honeycomb corrugation is only observed with the incident beam parallel to the zigzag direction while the geometric corrugation arising from the superlattice is revealed along the armchair direction. Full-quantum calculations of the diffraction patterns show the very high GIFAD sensitivity to the amplitude of the surface corrugation. The best agreement between the calculated and measuredmore » diffraction intensities yields a corrugation height of 0.27 ± 0.03 Å.« less

Electron coherent diffraction tomography of a nanocrystal

NASA Astrophysics Data System (ADS)

Dronyak, Roman; Liang, Keng S.; Tsai, Jin-Sheng; Stetsko, Yuri P.; Lee, Ting-Kuo; Chen, Fu-Rong

2010-05-01

Coherent diffractive imaging (CDI) with electron or x-ray sources is a promising technique for investigating the structure of nanoparticles down to the atomic scale. In electron CDI, a two-dimensional reconstruction is demonstrated using highly coherent illumination from a field-emission gun as a source of electrons. In a three-dimensional (3D) electron CDI, we experimentally determine the morphology of a single MgO nanocrystal using the Bragg diffraction geometry. An iterative algorithm is applied to invert the 3D diffraction pattern about a (200) reflection of the nanoparticle measured at an angular range of 1.8°. The results reveal a 3D image of the sample at ˜8 nm resolution, and agree with a simulation. Our work demonstrates an alternative approach to obtain the 3D structure of nanocrystals with an electron microscope.

Diffraction Correlation to Reconstruct Highly Strained Particles

NASA Astrophysics Data System (ADS)

Brown, Douglas; Harder, Ross; Clark, Jesse; Kim, J. W.; Kiefer, Boris; Fullerton, Eric; Shpyrko, Oleg; Fohtung, Edwin

2015-03-01

Through the use of coherent x-ray diffraction a three-dimensional diffraction pattern of a highly strained nano-crystal can be recorded in reciprocal space by a detector. Only the intensities are recorded, resulting in a loss of the complex phase. The recorded diffraction pattern therefore requires computational processing to reconstruct the density and complex distribution of the diffracted nano-crystal. For highly strained crystals, standard methods using HIO and ER algorithms are no longer sufficient to reconstruct the diffraction pattern. Our solution is to correlate the symmetry in reciprocal space to generate an a priori shape constraint to guide the computational reconstruction of the diffraction pattern. This approach has improved the ability to accurately reconstruct highly strained nano-crystals.

Diffraction data of core-shell nanoparticles from an X-ray free electron laser

DOE PAGES

Li, Xuanxuan; Chiu, Chun -Ya; Wang, Hsiang -Ju; ...

2017-04-11

X-ray free-electron lasers provide novel opportunities to conduct single particle analysis on nanoscale particles. Coherent diffractive imaging experiments were performed at the Linac Coherent Light Source (LCLS), SLAC National Laboratory, exposing single inorganic core-shell nanoparticles to femtosecond hard-X-ray pulses. Each facetted nanoparticle consisted of a crystalline gold core and a differently shaped palladium shell. Scattered intensities were observed up to about 7 nm resolution. Analysis of the scattering patterns revealed the size distribution of the samples, which is consistent with that obtained from direct real-space imaging by electron microscopy. Furthermore, scattering patterns resulting from single particles were selected and compiledmore » into a dataset which can be valuable for algorithm developments in single particle scattering research.« less

The crystal structure of paramagnetic copper(II) oxalate (CuC₂O₄): formation and thermal decomposition of randomly stacked anisotropic nano-sized crystallites.

PubMed

Christensen, Axel Nørlund; Lebech, Bente; Andersen, Niels Hessel; Grivel, Jean-Claude

2014-11-28

Synthetic copper(II) oxalate, CuC2O4, was obtained in a precipitation reaction between a copper(II) solution and an aqueous solution of oxalic acid. The product was identified from its conventional X-ray powder patterns which match that of the copper mineral Moolooite reported to have the composition CuC2O4·0.44H2O. Time resolved in situ investigations of the thermal decomposition of copper(II) oxalate using synchrotron X-ray powder diffraction showed that in air the compound converts to Cu2O at 215 °C and oxidizes to CuO at 345 °C. Thermo gravimetric analysis performed in an inert Ar-gas reveals that the material contains no crystal water and reduces to pure Cu at 295 °C. Magnetic susceptibility measurements in the temperature range from 2 K to 300 K show intriguing paramagnetic behaviour with no sign of magnetic order down to 2 K. A crystal structure investigation is made based on powder diffraction data using one neutron diffraction pattern obtained at 5 K (λ = 1.5949(1) Å) combined with one conventional and two synchrotron X-ray diffraction patterns obtained at ambient temperature using λ = 1.54056, 1.0981 and λ = 0.50483(1) Å, respectively. Based on the X-ray synchrotron data the resulting crystal structure is described in the monoclinic space group P2₁/c (#14) in the P12₁/n1 setting with unit cell parameters a = 5.9598(1) Å, b = 5.6089(1) Å, c = 5.1138 (1) Å, β = 115.320(1)°. The composition is CuC2O4 with atomic coordinates determined by FullProf refinement of the neutron diffraction data. The crystal structure consists of a random stacking of CuC2O4 micro-crystallites where half the Cu-atoms are placed at (2a) and the other half at (2b) positions with the corresponding oxalate molecules centred around the corresponding (2b) and (2a) site positions, respectively. The diffraction patterns obtained for both kinds of radiation show considerable broadening of several Bragg peaks caused by highly anisotropic microstructural size and strain effects. In contrast to the water reported to be present in Moolooite, neither thermogravimetric nor the in situ thermal decomposition investigations and crystal structure analysis of the neutron diffraction data revealed any trace of water. An appendix contains details about the profile parameters for the diffractometers used at the European Synchrotron Radiation Facility and the Institute Max von Laue-Paul Langevin.

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

DOE PAGES

Zhang, C.; Balachandran, S.; Eisenlohr, P.; ...

2017-10-04

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

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

Zhang, C.; Balachandran, S.; Eisenlohr, P.

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

Buckskin Drill Hole and CheMin X-ray Diffraction

NASA Image and Video Library

2015-12-17

The graph at right presents information from the NASA Curiosity Mars rover's onboard analysis of rock powder drilled from the "Buckskin" target location, shown at left. X-ray diffraction analysis of the Buckskin sample inside the rover's Chemistry and Mineralogy (CheMin) instrument revealed the presence of a silica-containing mineral named tridymite. This is the first detection of tridymite on Mars. Peaks in the X-ray diffraction pattern are from minerals in the sample, and every mineral has a diagnostic set of peaks that allows identification. The image of Buckskin at left was taken by the rover's Mars Hand Lens Imager (MAHLI) camera on July 30, 2015, and is also available at PIA19804. http://photojournal.jpl.nasa.gov/catalog/PIA20271

Three-dimensional imaging of nanoscale materials by using coherent x-rays

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

Miao, Jianwei

X-ray crystallography is currently the primary methodology used to determine the 3D structure of materials and macromolecules. However, many nanostructures, disordered materials, biomaterials, hybrid materials and biological specimens are noncrystalline and, hence, their structures are not accessible by X-ray crystallography. Probing these structures therefore requires the employment of different approaches. A very promising technique currently under rapid development is X-ray diffraction microscopy (or lensless imaging), in which the coherent X-ray diffraction pattern of a noncrystalline specimen is measured and then directly phased to obtain a high-resolution image. Through the DOE support over the past three years, we have applied X-raymore » diffraction microscopy to quantitative imaging of GaN quantum dot particles, and revealed the internal GaN-Ga2O3 core shell structure in three dimensions. By exploiting the abrupt change in the scattering cross-section near electronic resonances, we carried out the first experimental demonstration of resonant X-ray diffraction microscopy for element specific imaging. We performed nondestructive and quantitative imaging of buried Bi structures inside a Si crystal by directly phasing coherent X-ray diffraction patterns acquired below and above the Bi M5 edge. We have also applied X-ray diffraction microscopy to nondestructive imaging of mineral crystals inside biological composite materials - intramuscular fish bone - at the nanometer scale resolution. We identified mineral crystals in collagen fibrils at different stages of mineralization and proposed a dynamic mechanism to account for the nucleation and growth of mineral crystals in the collagen matrix. In addition, we have also discovered a novel 3D imaging modality, denoted ankylography, which allows for complete 3D structure determination without the necessity of sample titling or scanning. We showed that when the diffraction pattern of a finite object is sampled at a sufficiently fine scale on the Ewald sphere, the 3D structure of the object is determined by the 2D spherical pattern. We confirmed the theoretical analysis by performing 3D numerical reconstructions of a sodium silicate glass structure at 2 A resolution from a 2D spherical diffraction pattern alone. As X-ray free electron lasers are under rapid development worldwide, ankylography may open up a new horizon to obtain the 3D structure of a non-crystalline specimen from a single pulse and allow time-resolved 3D structure determination of disordered materials.« 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.

Synthesis and structural properties of Ba(1-x)LaxTiO3 perovskite nanoparticles fabricated by solvothermal synthesis route

NASA Astrophysics Data System (ADS)

Puli, Venkata Sreenivas; Adireddy, Shiva; Elupula, Ravinder; Molugu, Sudheer; Shipman, Josh; Chrisey, Douglas B.

2017-05-01

We report the successful synthesis and structural characterization of barium lanthanum titanate Ba(1-x)LaxTiO3 (x=0.003,0.006,0.010) nanoparticles. The colloidal nanoparticles were prepared with high yield by a solvothermal method at temperatures as low as 150°C for 24h. The as-prepared nanopowders were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. The XRD studies revealed pseudo-cubic crystalline structure, with no impurity phases at room temperature. However ferroelectric tetragonal modes were clearly observed using Raman spectroscopy measurements. From TEM measurements, uniformly sized BLT nanoparticles were observed. Selected area diffraction TEM images revealed polycrystalline perovskite ring patterns, identified as corresponding to the tetragonal phase.

First-principles prediction of low-energy structures for AlH3

NASA Astrophysics Data System (ADS)

Sun, Shoutian; Ke, Xuezhi; Chen, Changfeng; Tanaka, Isao

2009-01-01

We report density-functional calculations that predict ten different low-energy structures for aluminum hydride AlH3 with space groups Pnma , P6/mmm , I4/mcm , P4/mbm , P4/nmm , Pm3¯m , P21/m , P21/c , Pbcm , and P4/n . Phonon calculations within harmonic approximation reveal unstable modes in the P6/mmm , I4/mcm , P4/mbm , P4/nmm , Pm3¯m , P21/m , and P21/c structures, indicating that they are unstable at low temperatures. The calculations show that the thermodynamic stabilities for AlH3 with space groups Pnma , Pbcm , and P4/n are overall close to the existing α - and γ-AlH3 . From x-ray powder-diffraction patterns, the simulated main-peak positions for AlH3 (P4/n) are in good agreement with experimental δ-AlH3 . A full Rietveld analysis reveals that the fitting space groups R3¯c , Pbcm , and Pnma to the experimental x-ray powder-diffraction pattern of α-AlH3 gives almost the same satisfactory result.

Signal enhancement and Patterson-search phasing for high-spatial-resolution coherent X-ray diffraction imaging of biological objects.

PubMed

Takayama, Yuki; Maki-Yonekura, Saori; Oroguchi, Tomotaka; Nakasako, Masayoshi; Yonekura, Koji

2015-01-28

In this decade coherent X-ray diffraction imaging has been demonstrated to reveal internal structures of whole biological cells and organelles. However, the spatial resolution is limited to several tens of nanometers due to the poor scattering power of biological samples. The challenge is to recover correct phase information from experimental diffraction patterns that have a low signal-to-noise ratio and unmeasurable lowest-resolution data. Here, we propose a method to extend spatial resolution by enhancing diffraction signals and by robust phasing. The weak diffraction signals from biological objects are enhanced by interference with strong waves from dispersed colloidal gold particles. The positions of the gold particles determined by Patterson analysis serve as the initial phase, and this dramatically improves reliability and convergence of image reconstruction by iterative phase retrieval. A set of calculations based on current experiments demonstrates that resolution is improved by a factor of two or more.

Signal enhancement and Patterson-search phasing for high-spatial-resolution coherent X-ray diffraction imaging of biological objects

PubMed Central

Takayama, Yuki; Maki-Yonekura, Saori; Oroguchi, Tomotaka; Nakasako, Masayoshi; Yonekura, Koji

2015-01-01

In this decade coherent X-ray diffraction imaging has been demonstrated to reveal internal structures of whole biological cells and organelles. However, the spatial resolution is limited to several tens of nanometers due to the poor scattering power of biological samples. The challenge is to recover correct phase information from experimental diffraction patterns that have a low signal-to-noise ratio and unmeasurable lowest-resolution data. Here, we propose a method to extend spatial resolution by enhancing diffraction signals and by robust phasing. The weak diffraction signals from biological objects are enhanced by interference with strong waves from dispersed colloidal gold particles. The positions of the gold particles determined by Patterson analysis serve as the initial phase, and this dramatically improves reliability and convergence of image reconstruction by iterative phase retrieval. A set of calculations based on current experiments demonstrates that resolution is improved by a factor of two or more. PMID:25627480

Fast switchable ferroelectric liquid crystal gratings with two electro-optical modes

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

Ma, Ying; Srivastava, A. K., E-mail: abhishek-srivastava-lu@yahoo.co.in; Chigrinov, V. G.

In this article, we reveal a theoretical and experimental illustration of the Ferroelectric liquid crystal (FLC) grating fabricated by mean of patterned alignment based on photo-alignment. The complexity related to the mismatching of the predefined alignment domains on the top and bottom substrate has been avoided by incorporating only one side photo aligned substrate while the other substrate does not have any alignment layer. Depending on the easy axis in the said alignment domains and the azimuth plane of the impinging polarized light, the diffracting element can be tuned in two modes i.e. DIFF/OFF switchable and DIFF/TRANS switchable modes, whichmore » can be applied to different applications. The diffraction profile has been illustrated theoretically that fits well with the experimental finding and thus the proposed diffraction elements with fast response time and high diffraction efficiency could find application in many modern devices.« less

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

Network based approaches reveal clustering in protein point patterns

NASA Astrophysics Data System (ADS)

Parker, Joshua; Barr, Valarie; Aldridge, Joshua; Samelson, Lawrence E.; Losert, Wolfgang

2014-03-01

Recent advances in super-resolution imaging have allowed for the sub-diffraction measurement of the spatial location of proteins on the surfaces of T-cells. The challenge is to connect these complex point patterns to the internal processes and interactions, both protein-protein and protein-membrane. We begin analyzing these patterns by forming a geometric network amongst the proteins and looking at network measures, such the degree distribution. This allows us to compare experimentally observed patterns to models. Specifically, we find that the experimental patterns differ from heterogeneous Poisson processes, highlighting an internal clustering structure. Further work will be to compare our results to simulated protein-protein interactions to determine clustering mechanisms.

Magneto-structural studies of sol-gel synthesized nanocrystalline manganese substituted nickel ferrites

NASA Astrophysics Data System (ADS)

Pandav, R. S.; Patil, R. P.; Chavan, S. S.; Mulla, I. S.; Hankare, P. P.

2016-11-01

Nanocrystalline NiFe2-xMnxO4 (2≥x≥0) ferrites were prepared by sol-gel method. X-ray diffraction patterns reveal that synthesized compounds are in single phase cubic spinel lattice for all the composition. The surface morphology of all the samples were studied by scanning electron microscopy. The particle size measured from transmission electron microscopy and X-ray diffraction patterns confirms the nanosized dimension of the as-prepared powder. The elemental analysis was carried out by energy dispersive X-ray analysis technique. Magnetic properties such as saturation magnetization, coercivity and remanence are studied as a function of increasing Mn concentration at room temperature. The saturation magnetization shows a decreasing trend with increase in Mn content. The substitution of manganese in the nickel ferrite affects the structural and magnetic properties of cubic spinels.

Grain rotation and lattice deformation during photoinduced chemical reactions revealed by in situ X-ray nanodiffraction.

PubMed

Huang, Zhifeng; Bartels, Matthias; Xu, Rui; Osterhoff, Markus; Kalbfleisch, Sebastian; Sprung, Michael; Suzuki, Akihiro; Takahashi, Yukio; Blanton, Thomas N; Salditt, Tim; Miao, Jianwei

2015-07-01

In situ X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to investigate many physical science phenomena, ranging from phase transitions, chemical reactions and crystal growth to grain boundary dynamics. A major limitation of in situ XRD and TEM is a compromise that has to be made between spatial and temporal resolution. Here, we report the development of in situ X-ray nanodiffraction to measure high-resolution diffraction patterns from single grains with up to 5 ms temporal resolution. We observed, for the first time, grain rotation and lattice deformation in chemical reactions induced by X-ray photons: Br(-) + hv → Br + e(-) and e(-) + Ag(+) → Ag(0). The grain rotation and lattice deformation associated with the chemical reactions were quantified to be as fast as 3.25 rad s(-1) and as large as 0.5 Å, respectively. The ability to measure high-resolution diffraction patterns from individual grains with a temporal resolution of several milliseconds is expected to find broad applications in materials science, physics, chemistry and nanoscience.

Near-surface density profiling of Fe ion irradiated Si (100) using extremely asymmetric x-ray diffraction by variation of the wavelength

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

Khanbabaee, B., E-mail: khanbabaee@physik.uni-siegen.de; Pietsch, U.; Facsko, S.

2014-10-20

In this work, we report on correlations between surface density variations and ion parameters during ion beam-induced surface patterning process. The near-surface density variations of irradiated Si(100) surfaces were investigated after off-normal irradiation with 5 keV Fe ions at different fluences. In order to reduce the x-ray probing depth to a thickness below 5 nm, the extremely asymmetrical x-ray diffraction by variation of wavelength was applied, exploiting x-ray refraction at the air-sample interface. Depth profiling was achieved by measuring x-ray rocking curves as function of varying wavelengths providing incidence angles down to 0°. The density variation was extracted from the deviationsmore » from kinematical Bragg angle at grazing incidence angles due to refraction of the x-ray beam at the air-sample interface. The simulations based on the dynamical theory of x-ray diffraction revealed that while a net near-surface density decreases with increasing ion fluence which is accompanied by surface patterning, there is a certain threshold of ion fluence to surface density modulation. Our finding suggests that the surface density variation can be relevant with the mechanism of pattern formation.« less

Paper surface diffraction to characterize the fiber orientation distribution

NASA Astrophysics Data System (ADS)

Pereira, Mario; Teixeira, Jose; Fiadeiro, Paulo T.; Silvy, Jacques

2001-11-01

Many paper mills use ultrasonic techniques to measure the Tensile Stiffness Index, TSI, of the paper sheet. They then assume that the TSI value is the same as the fibre orientation anisotropy. This is true if the paper is allowed to dry without any internal tension or elongation, but does not apply to paper manufactured in a paper machine. The paper machine introduces tension and elongation as soon as the fibre is placed on the forming fabric. These factors increase through the press section and are accentuated in the drying section. In order to uniquely measure the fibre orientation anisotropy on the surfaces, the proposed method uses replicas of both paper surfaces to produce a laser diffraction pattern. The obtained pattern reveals an elliptical shape, which is related to the fibre orientation anisotropy of the paper surface. By measuring the ellipticity of the diffraction pattern and the deviation with respect to the machine direction, one can quantify the fibre orientation distribution. Different papers from the bench market have been successfully tested with the developed system. This article describes the new developed optical system and its innovative capabilities in the field to produce maps of the fibre orientation of a complete paper sheet surface. A selection of the obtained results to prove its feasibility is also presented.

Effect of gamma-irradiation on thermal decomposition kinetics, X-ray diffraction pattern and spectral properties of tris(1,2-diaminoethane)nickel(II)sulphate

NASA Astrophysics Data System (ADS)

Jayashri, T. A.; Krishnan, G.; Rema Rani, N.

2014-12-01

Tris(1,2-diaminoethane)nickel(II)sulphate was prepared, and characterised by various chemical and spectral techniques. The sample was irradiated with 60Co gamma rays for varying doses. Sulphite ion and ammonia were detected and estimated in the irradiated samples. Non-isothermal decomposition kinetics, X-ray diffraction pattern, Fourier transform infrared spectroscopy, electronic, fast atom bombardment mass spectra, and surface morphology of the complex were studied before and after irradiation. Kinetic parameters were evaluated by integral, differential, and approximation methods. Irradiation enhanced thermal decomposition, lowering thermal and kinetic parameters. The mechanism of decomposition is controlled by R3 function. From X-ray diffraction studies, change in lattice parameters and subsequent changes in unit cell volume and average crystallite size were observed. Both unirradiated and irradiated samples of the complex belong to trigonal crystal system. Decrease in the intensity of the peaks was observed in the infrared spectra of irradiated samples. Electronic spectral studies revealed that the M-L interaction is unaffected by irradiation. Mass spectral studies showed that the fragmentation patterns of the unirradiated and irradiated samples are similar. The additional fragment with m/z 256 found in the irradiated sample is attributed to S8+. Surface morphology of the complex changed upon irradiation.

Simultaneous multiscale measurements on dynamic deformation of a magnesium alloy with synchrotron x-ray imaging and diffraction

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

Lu, L.; Sun, T.; Fezzaa, K.

Dynamic split Hopkinson pressure bar experiments with in situ synchrotron x-ray imaging and diffraction are conducted on a rolled magnesium alloy at high strain rates of ~5500 s-1. High speed multiscale measurements including stress–strain curves (macroscale), strain fields (mesoscale), and diffraction patterns (microscale) are obtained simultaneously, revealing strong anisotropy in deformation across different length scales. {1012} extension twinning induces homogenized strain fields and gives rise to rapid increase in strain hardening rate, while dislocation motion leads to inhomogeneous deformation and a decrease in strain hardening rate. During the early stage of plastic deformation, twinning is dominant in dynamic compression, whilemore » dislocation motion prevails in quasi-static loading, manifesting a strain-rate dependence of deformation.« less

Brominated carbon black: An EDXD study

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

Carbone, Marilena; Gontrani, Lorenzo, E-mail: lorenzo.gontrani@uniroma1.it

2014-06-19

An energy dispersive X-Ray study of pure and brominated carbon black was carried out. The analysis of the diffraction patterns reveals that the low bromine load (ca.1% mol) is trapped into the structure, without significantly modifying it. This allows the application of the difference methods, widely tested for electrolyte solutions, inorganic matrices containing metals and isomorphic substitutions.

Computer Generated Diffraction Patterns Of Rough Surfaces

NASA Astrophysics Data System (ADS)

Rakels, Jan H.

1989-03-01

It is generally accepted, that optical methods are the most promising for the in-process measurement of surface finish. These methods have the advantages of being non-contacting and fast data acquisition. In the Micro-Engineering Centre at the University of Warwick, an optical sensor has been devised which can measure the rms roughness, slope and wavelength of turned and precision ground surfaces. The operation of this device is based upon the Kirchhoff-Fresnel diffraction integral. Application of this theory to ideal turned surfaces is straightforward, and indeed the theoretically calculated diffraction patterns are in close agreement with patterns produced by an actual optical instrument. Since it is mathematically difficult to introduce real surface profiles into the diffraction integral, a computer program has been devised, which simulates the operation of the optical sensor. The program produces a diffraction pattern as a graphical output. Comparison between computer generated and actual diffraction patterns of the same surfaces show a high correlation.

Diffractive elements for generating microscale laser beam patterns: a Y2K problem

NASA Astrophysics Data System (ADS)

Teiwes, Stephan; Krueger, Sven; Wernicke, Guenther K.; Ferstl, Margit

2000-03-01

Lasers are widely used in industrial fabrication for engraving, cutting and many other purposes. However, material processing at very small scales is still a matter of concern. Advances in diffractive optics could provide for laser systems that could be used for engraving or cutting of micro-scale patterns at high speeds. In our paper we focus on the design of diffractive elements which can be used for this special application. It is a common desire in material processing to apply 'discrete' as well as 'continuous' beam patterns. Especially, the latter case is difficult to handle as typical micro-scale patterns are characterized by bad band-limitation properties, and as speckles can easily occur in beam patterns. It is shown in this paper that a standard iterative design method usually fails to obtain diffractive elements that generate diffraction patterns with acceptable quality. Insights gained from an analysis of the design problems are used to optimize the iterative design method. We demonstrate applicability and success of our approach by the design of diffractive phase elements that generate a discrete and a continuous 'Y2K' pattern.

High Pressure X-Ray Diffraction Studies of Nanocrystalline Materials

NASA Technical Reports Server (NTRS)

Palosz, B.; Stel'makh, S.; Grzanka, E.; Gierlotka, S.; Palosz, W.

2004-01-01

Experimental evidence obtained for a variety of nanocrystalline materials suggest that the crystallographic structure of a very small size particle deviates from that in the bulk crystals. In this paper we show the effect of the surface of nanocrystals on their structure by the analysis of generation and distribution of macro- and micro-strains at high pressures and their dependence on the grain size in nanocrystalline powders of Sic. We studied the structure of Sic nanocrystals by in-situ high-pressure powder diffraction technique using synchrotron and neutron sources and hydrostatic or isostatic pressure conditions. The diffraction measurements were done in HASYLAB at DESY using a Diamond Anvil Cell (DAC) in the energy dispersive geometry in the diffraction vector range up to 3.5 - 4/A and under pressures up to 50 GPa at room temperature. In-situ high pressure neutron diffraction measurements were done at LANSCE in Los Alamos National Laboratory using the HIPD and HIPPO diffractometers with the Paris-Edinburgh and TAP-98 cells, respectively, in the diffraction vector range up to 26 Examination of the response of the material to external stresses requires nonstandard methodology of the materials characterization and description. Although every diffraction pattern contains a complete information on macro- and micro-strains, a high pressure experiment can reveal only those factors which contribute to the characteristic diffraction patterns of the crystalline phases present in the sample. The elastic properties of powders with the grain size from several nm to micrometers were examined using three methodologies: (l), the analysis of positions and widths of individual Bragg reflections (used for calculating macro- and micro-strains generated during densification) [I], (2). the analysis of the dependence of the experimental apparent lattice parameter, alp, on the diffraction vector Q [2], and (3), the atomic Pair Distribution Function (PDF) technique [3]. The results of our studies show, that Sic nanocrystals have the features of two phases, each with its distinct elastic properties. and under pressures up to 8 GPa.

Coherent diffraction imaging: consistency of the assembled three-dimensional distribution.

PubMed

Tegze, Miklós; Bortel, Gábor

2016-07-01

The short pulses of X-ray free-electron lasers can produce diffraction patterns with structural information before radiation damage destroys the particle. From the recorded diffraction patterns the structure of particles or molecules can be determined on the nano- or even atomic scale. In a coherent diffraction imaging experiment thousands of diffraction patterns of identical particles are recorded and assembled into a three-dimensional distribution which is subsequently used to solve the structure of the particle. It is essential to know, but not always obvious, that the assembled three-dimensional reciprocal-space intensity distribution is really consistent with the measured diffraction patterns. This paper shows that, with the use of correlation maps and a single parameter calculated from them, the consistency of the three-dimensional distribution can be reliably validated.

Single-Slit Diffraction Pattern of a Thermal Atomic Potassium Beam

ERIC Educational Resources Information Center

Leavitt, John A.; Bills, Francis A.

1969-01-01

The diffraction of a full thermal atomic potassium beam by a single slit was observed. Four experimental diffraction patterns were compared with that predicted by de Brogtie's hypothesis and simple scalar Fresnel diffraction theory. Possible reasons for the differences were discussed. (LC)

Understanding Inhomogeneous Reactions in Li‐Ion Batteries: Operando Synchrotron X‐Ray Diffraction on Two‐Layer Electrodes

PubMed Central

Villevieille, Claire; Takeuchi, Yoji

2015-01-01

To understand inhomogeneous reactions perpendicular to the current collector in an electrode for batteries, a method combining operando synchrotron X‐ray diffraction and two‐layer electrodes with different porosities is developed. The two layers are built using two different active materials (LiNi0.80Co0.15Al0.05O2 and LiMn2O4), therefore, tracing each diffraction pattern reveals which active material is reacting during the electrochemical measurement in transmission mode. The results demonstrate that the active material close to the separator is obviously more active than that one close to the current collector in the case of low porosity electrodes. This inhomogeneity should be due to the rate‐limitation and especially to low average ionic conductivity of the electrolyte in the porous electrode because the current flows first mainly into the electrode regions close to the separator. The inhomogeneity is found to be mitigated by the adjustment of the electrode density and thus porosity. Hence, the novel operando method reveals a clear inhomogeneous reaction perpendicular to the current collector. PMID:27708998

Time-resolved x-ray imaging of a laser-induced nanoplasma and its neutral residuals

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

Fluckiger, L.; Rupp, D.; Adolph, M.

The evolution of individual, large gas-phase xenon clusters, turned into a nanoplasma by a high power infrared laser pulse, is tracked from femtoseconds up to nanoseconds after laser excitation via coherent diffractive imaging, using ultra-short soft x-ray free electron laser pulses. A decline of scattering signal at high detection angles with increasing time delay indicates a softening of the cluster surface. Here we demonstrate, for the first time a representative speckle pattern of a new stage of cluster expansion for xenon clusters after a nanosecond irradiation. The analysis of the measured average speckle size and the envelope of the intensitymore » distribution reveals a mean cluster size and length scale of internal density fluctuations. Furthermore, the measured diffraction patterns were reproduced by scattering simulations which assumed that the cluster expands with pronounced internal density fluctuations hundreds of picoseconds after excitation.« less

Time-resolved x-ray imaging of a laser-induced nanoplasma and its neutral residuals

DOE PAGES

Fluckiger, L.; Rupp, D.; Adolph, M.; ...

2016-04-13

The evolution of individual, large gas-phase xenon clusters, turned into a nanoplasma by a high power infrared laser pulse, is tracked from femtoseconds up to nanoseconds after laser excitation via coherent diffractive imaging, using ultra-short soft x-ray free electron laser pulses. A decline of scattering signal at high detection angles with increasing time delay indicates a softening of the cluster surface. Here we demonstrate, for the first time a representative speckle pattern of a new stage of cluster expansion for xenon clusters after a nanosecond irradiation. The analysis of the measured average speckle size and the envelope of the intensitymore » distribution reveals a mean cluster size and length scale of internal density fluctuations. Furthermore, the measured diffraction patterns were reproduced by scattering simulations which assumed that the cluster expands with pronounced internal density fluctuations hundreds of picoseconds after excitation.« less

Silica in Opal at Buckskin and Greenhorn on Mount Sharp

NASA Image and Video Library

2015-12-17

This graph presents information from the NASA Curiosity Mars rover's onboard analysis of rock powder drilled from the "Buckskin" and "Greenhorn" target locations on lower Mount Sharp. Buckskin, in the "Marias Pass" area, and Greenhorn, in the "Bridger Basin" area, both contain high concentrations of silica. X-ray diffraction analysis of powered samples inside Curiosity's Chemistry and Mineralogy (CheMin) instrument revealed that each of them contains silica in the form of noncrystalline opal. The broad hump in the two X-ray diffraction patterns is diagnostic of opaline silica. Some of the silica in Buckskin is in the form of tridymite. http://photojournal.jpl.nasa.gov/catalog/PIA20273

Phyllotactic arrangements of optical elements

NASA Astrophysics Data System (ADS)

Horacek, M.; Meluzin, P.; Kratky, S.; Matejka, M.; Kolarik, V.

2017-05-01

Phyllotaxy studies arrangements of biological entities, e.g. a placement of seeds in the flower head. Vogel (1979) presented a phyllotactic model based on series of seeds ordered along a primary spiral. This arrangement allows each seed to occupy the same area within a circular flower head. Recently, a similar arrangement of diffraction primitives forming a planar relief diffractive structure was presented. The planar relief structure was used for benchmarking and testing purposes of the electron beam writer patterning process. This contribution presents the analysis of local periods and azimuths of optical phyllotactic arrangements. Two kinds of network characteristic triangles are introduced. If the discussed planar structure has appropriate size and density, diffraction of the incoming light creates characteristic a phyllotactic diffraction pattern. Algorithms enabling the analysis of such behavior were developed and they were validated by fabricated samples of relief structures. Combined and higher diffraction orders are also analyzed. Different approaches enabling the creation of phyllotactic diffractive patterns are proposed. E-beam lithography is a flexible technology for various diffraction gratings origination. The e-beam patterning typically allows for the creation of optical diffraction gratings in the first diffraction order. Nevertheless, this technology enables also more complex grating to be prepared, e.g. blazed gratings and zero order gratings. Moreover, the mentioned kinds of gratings can be combined within one planar relief structure. The practical part of the presented work deals with the nano patterning of such structures by using two different types of the e-beam pattern generators.

Predicted and measured transmission and diffraction by a metallic mesh coating

NASA Astrophysics Data System (ADS)

Halman, Jennifer I.; Ramsey, Keith A.; Thomas, Michael; Griffin, Andrew

2009-05-01

Metallic mesh coatings are used on visible and infrared windows and domes to provide shielding from electromagnetic interference (EMI) and as heaters to de-fog or de-ice windows or domes. The periodic metallic mesh structures that provide the EMI shielding and/or resistive electrical paths for the heating elements create a diffraction pattern when optical or infrared beams are incident on the coated windows. Over the years several different mesh geometries have been used to try to reduce the effects of diffraction. We have fabricated several different mesh patterns on small coupons of BK-7 and measured the transmitted power and the diffraction patterns of each one using a CW 1064 nm laser. In this paper we will present some predictions and measurements of the diffraction patterns of several different mesh patterns.

Table of interplanar spacings for crystal-structure determinations by X-ray diffraction with molybdenum, copper, cobalt, iron, and chromium radiations

NASA Technical Reports Server (NTRS)

Kittel, J Howard

1945-01-01

For a simple diffraction pattern, the time required to calculate interplanar distances from measurements of the pattern is not excessive. If more than a few lines are present, however, or if several patterns are to be studied, it is very advantageous to have available a table giving interplanar spacings directly in terms of the linear measurements made on the film of the lines appearing on the diffraction pattern. The preparation of the table given here was undertaken when the expansion of research activities involving X-ray diffraction techniques indicated that such a table would greatly decrease the time required to analyze diffraction patterns. The table was prepared for use with K alpha(sub 1) radiation from the following target materials: molybdenum, copper, cobalt, iron, and chromium.

Visible diffraction from quasi-crystalline arrays of carbon nanotubes

NASA Astrophysics Data System (ADS)

Butler, Timothy P.; Butt, Haider; Wilkinson, Timothy D.; Amaratunga, Gehan A. J.

2015-08-01

Large area arrays of vertically-aligned carbon nanotubes (VACNTs) are patterned in a quasi-crystalline Penrose tile arrangement through electron beam lithography definition of Ni catalyst dots and subsequent nanotube growth by plasma-enhanced chemical vapour deposition. When illuminated with a 532 nm laser beam high-quality and remarkable diffraction patterns are seen. The diffraction is well matched to theoretical calculations which assume apertures to be present at the location of the VACNTs for transmitted light. The results show that VACNTs act as diffractive elements in reflection and can be used as spatially phased arrays for producing tailored diffraction patterns.

Orientation Dependence of the Deformation Microstructure of Ta-4%W after Cold-Rolling

NASA Astrophysics Data System (ADS)

Zhang, J.; Ma, G. Q.; Godfrey, A.; Shu, D. Y.; Chen, Q.; Wu, G. L.

2017-07-01

One of the common features of deformed face-centered cubic metals with medium to high stacking fault energy is the formation of geometrically necessary dislocation boundaries. The dislocation boundary arrangements in refractory metals with body-centered cubic crystal structure are, however, less well known. To address this issue a Ta-4%W alloy was cold rolled up to 70% in thickness in the present work. The resulting deformation microstructures were characterized by electron back-scattering diffraction and the dislocation boundary arrangements in each grain were revealed using sample-frame misorientation axis maps calculated using an in-house code. The maps were used to analyze the slip pattern of individual grains after rolling, revealing an orientation dependence of the slip pattern.

Microscopic evolution of dielectric nanoparticles at different calcination temperatures synthesized via sol-gel auto-combustion

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

Adil, Muhammad, E-mail: muhammadadil86@hotmail.com; Zaid, Hasnah Mohd, E-mail: hasnamz@petronas.com.my; Chuan, Lee Kean, E-mail: lee.kc@petronas.com.my

2015-07-22

Dielectric nano powder synthesis is carried by a simple and fast sol-gel auto-combustion method. The transformation of crystalline phases of as-synthesized nano powders is investigated through the detailed transmission electron microscopy (TEM), revealed the crystallographic alterations and morphological information even at lattice scale. From specific area electron diffraction (SAED) pattern, has specified the d-spacing and corresponding planes supported by the observed lattice fringes. The morphological characterization of nanoparticles is performed through field-emission scanning electron microscopy (FESEM), exhibiting the increment in particle size due to agglomeration with the increase in annealing temperature. Furthermore, EDX pattern has been used to verify themore » formation of nanoparticles by revealing the presence of required elements.« less

SU-E-I-77: X-Ray Coherent Scatter Diffraction Pattern Modeling in GEANT4.

PubMed

Kapadia, A; Samei, E; Harrawood, B; Sahbaee, P; Chawla, A; Tan, Z; Brady, D

2012-06-01

To model X-ray coherent scatter diffraction patterns in GEANT4 for simulating experiments involving material detection through diffraction pattern measurement. Although coherent scatter cross-sections are modeled accurately in GEANT4, diffraction patterns for crystalline materials are not yet included. Here we describe our modeling of crystalline diffraction patterns in GEANT4 for specific materials and the validation of the results against experimentally measured data. Coherent scatter in GEANT4 is currently based on Hubbell's non-relativistic form factor tabulations from EPDL97. We modified the form-factors by introducing an interference function that accounts for the angular dependence between the Rayleigh-scattered photons and the photon wavelength. The modified form factors were used to replace the inherent form-factors in GEANT4. The simulation was tested using monochromatic and polychromatic x-ray beams (separately) incident on objects containing one or more elements with modified form-factors. The simulation results were compared against the experimentally measured diffraction images of corresponding objects using an in-house x-ray diffraction imager for validation. The comparison was made using the following metrics: number of diffraction rings, radial distance, absolute intensity, and relative intensity. Sharp diffraction pattern rings were observed in the monochromatic simulations at locations consistent with the angular dependence of the photon wavelength. In the polychromatic simulations, the diffraction patterns exhibited a radial blur consistent with the energy spread of the polychromatic spectrum. The simulated and experimentally measured patterns showed identical numbers of rings with close agreement in radial distance, absolute and relative intensities (barring statistical fluctuations). No significant change was observed in the execution time of the simulations. This work demonstrates the ability to model coherent scatter diffraction in GEANT4 in an accurate and efficient manner without compromising the accuracy or runtime of the simulation. This work was supported by the Department of Homeland Security under grant DHS (BAA 10-01 F075), and by the Department of Defense under award W81XWH-09-1-0066. © 2012 American Association of Physicists in Medicine.

Light diffraction studies of single muscle fibers as a function of fiber rotation.

PubMed Central

Gilliar, W G; Bickel, W S; Bailey, W F

1984-01-01

Light diffraction patterns from single glycerinated frog semitendinosus muscle fibers were examined photographically and photoelectrically as a function of diffraction angle and fiber rotation. The total intensity diffraction pattern indicates that the order maxima change both position and intensity periodically as a function of rotation angle. The total diffracted light, light diffracted above and below the zero-order plane, and light diffracted into individual orders gives information about the fiber's longitudinal and rotational structure and its noncylindrical symmetry. Images FIGURE 2 PMID:6611174

Annealing effect on thermal conductivity and microhardness of carbon nanotube containing Se80Te16Cu4 glassy composites

NASA Astrophysics Data System (ADS)

Upadhyay, A. N.; Tiwari, R. S.; Singh, Kedar

2018-02-01

This study deals with the effect of thermal annealing on structural/microstructural, thermal and mechanical behavior of pristine Se80Te16Cu4 and carbon nanotubes (CNTs) containing Se80Te16Cu4 glassy composites. Pristine Se80Te16Cu4, 3 and 5 wt%CNTs-Se80Te16Cu4 glassy composites are annealed in the vicinity of glass transition temperature to onset crystallization temperature (340-380 K). X-ray diffraction (XRD) pattern revealed formation of polycrystalline phases of hexagonal CuSe and trigonal selenium. The indexed d-values in XRD patterns are in well conformity with the d-values obtained after the indexing of the ring pattern of selected area electron diffraction pattern of TEM images. The SEM investigation exhibited that the grain size of the CNTs containing Se80Te16Cu4 glassy composites increased with increasing annealing temperature and decreased at further higher annealing temperature. Thermal conductivity, microhardness exhibited a substantial increase with increasing annealing temperature of 340-360 K and slightly decreases for 380 K. The variation of thermal conductivity and microhardness can be explained by cross-linking formation and voids reduction.

High throughput screening of ligand binding to macromolecules using high resolution powder diffraction

DOEpatents

Von Dreele, Robert B.; D'Amico, Kevin

2006-10-31

A process is provided for the high throughput screening of binding of ligands to macromolecules using high resolution powder diffraction data including producing a first sample slurry of a selected polycrystalline macromolecule material and a solvent, producing a second sample slurry of a selected polycrystalline macromolecule material, one or more ligands and the solvent, obtaining a high resolution powder diffraction pattern on each of said first sample slurry and the second sample slurry, and, comparing the high resolution powder diffraction pattern of the first sample slurry and the high resolution powder diffraction pattern of the second sample slurry whereby a difference in the high resolution powder diffraction patterns of the first sample slurry and the second sample slurry provides a positive indication for the formation of a complex between the selected polycrystalline macromolecule material and at least one of the one or more ligands.

Femtosecond X-ray coherent diffraction of aligned amyloid fibrils on low background graphene.

PubMed

Seuring, Carolin; Ayyer, Kartik; Filippaki, Eleftheria; Barthelmess, Miriam; Longchamp, Jean-Nicolas; Ringler, Philippe; Pardini, Tommaso; Wojtas, David H; Coleman, Matthew A; Dörner, Katerina; Fuglerud, Silje; Hammarin, Greger; Habenstein, Birgit; Langkilde, Annette E; Loquet, Antoine; Meents, Alke; Riek, Roland; Stahlberg, Henning; Boutet, Sébastien; Hunter, Mark S; Koglin, Jason; Liang, Mengning; Ginn, Helen M; Millane, Rick P; Frank, Matthias; Barty, Anton; Chapman, Henry N

2018-05-09

Here we present a new approach to diffraction imaging of amyloid fibrils, combining a free-standing graphene support and single nanofocused X-ray pulses of femtosecond duration from an X-ray free-electron laser. Due to the very low background scattering from the graphene support and mutual alignment of filaments, diffraction from tobacco mosaic virus (TMV) filaments and amyloid protofibrils is obtained to 2.7 Å and 2.4 Å resolution in single diffraction patterns, respectively. Some TMV diffraction patterns exhibit asymmetry that indicates the presence of a limited number of axial rotations in the XFEL focus. Signal-to-noise levels from individual diffraction patterns are enhanced using computational alignment and merging, giving patterns that are superior to those obtainable from synchrotron radiation sources. We anticipate that our approach will be a starting point for further investigations into unsolved structures of filaments and other weakly scattering objects.

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.

A generalized method for high throughput in-situ experiment data analysis: An example of battery materials exploration

NASA Astrophysics Data System (ADS)

Aoun, Bachir; Yu, Cun; Fan, Longlong; Chen, Zonghai; Amine, Khalil; Ren, Yang

2015-04-01

A generalized method is introduced to extract critical information from series of ranked correlated data. The method is generally applicable to all types of spectra evolving as a function of any arbitrary parameter. This approach is based on correlation functions and statistical scedasticity formalism. Numerous challenges in analyzing high throughput experimental data can be tackled using the herein proposed method. We applied this method to understand the reactivity pathway and formation mechanism of a Li-ion battery cathode material during high temperature synthesis using in-situ high-energy X-ray diffraction. We demonstrate that Pearson's correlation function can easily unravel all major phase transition and, more importantly, the minor structural changes which cannot be revealed by conventionally inspecting the series of diffraction patterns. Furthermore, a two-dimensional (2D) reactivity pattern calculated as the scedasticity along all measured reciprocal space of all successive diffraction pattern pairs unveils clearly the structural evolution path and the active areas of interest during the synthesis. The methods described here can be readily used for on-the-fly data analysis during various in-situ operando experiments in order to quickly evaluate and optimize experimental conditions, as well as for post data analysis and large data mining where considerable amount of data hinders the feasibility of the investigation through point-by-point inspection.

A generalized method for high throughput in-situ experiment data analysis: An example of battery materials exploration

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

Aoun, Bachir; Yu, Cun; Fan, Longlong

A generalized method is introduced to extract critical information from series of ranked correlated data. The method is generally applicable to all types of spectra evolving as a function of any arbitrary parameter. This approach is based on correlation functions and statistical scedasticity formalism. Numerous challenges in analyzing high throughput experimental data can be tackled using the herein proposed method. We applied this method to understand the reactivity pathway and formation mechanism of a Li-ion battery cathode material during high temperature synthesis using in-situ highenergy X-ray diffraction. We demonstrate that Pearson's correlation function can easily unravel all major phase transitionmore » and, more importantly, the minor structural changes which cannot be revealed by conventionally inspecting the series of diffraction patterns. Furthermore, a two-dimensional (2D) reactivity pattern calculated as the scedasticity along all measured reciprocal space of all successive diffraction pattern pairs unveils clearly the structural evolution path and the active areas of interest during the synthesis. The methods described here can be readily used for on-the-fly data analysis during various in-situ operando experiments in order to quickly evaluate and optimize experimental conditions, as well as for post data analysis and large data mining where considerable amount of data hinders the feasibility of the investigation through point-by-point inspection.« less

Rietveld analysis of X-ray powder diffraction patterns as a potential tool for the identification of impact-deformed carbonate rocks

NASA Astrophysics Data System (ADS)

Huson, S. A.; Foit, F. F.; Watkinson, A. J.; Pope, M. C.

2009-12-01

Previous X-ray powder diffraction (XRD) studies revealed that shock deformed carbonates and quartz have broader XRD patterns than those of unshocked samples. Entire XRD patterns, single peak profiles and Rietveld refined parameters of carbonate samples from the Sierra Madera impact crater, west Texas, unshocked equivalent samples from 95 miles north of the crater and the Mission Canyon Formation of southwest Montana and western Wyoming were used to evaluate the use of X-ray powder diffraction as a potential tool for distinguishing impact deformed rocks from unshocked and tectonically deformed rocks. At Sierra Madera dolostone and limestone samples were collected from the crater rim (lower shock intensity) and the central uplift (higher shock intensity). Unshocked equivalent dolostone samples were collected from well cores drilled outside of the impact crater. Carbonate rocks of the Mission Canyon Formation were sampled along a transect across the tectonic front of the Sevier and Laramide orogenic belts. Whereas calcite subjected to significant shock intensities at the Sierra Madera impact crater can be differentiated from tectonically deformed calcite from the Mission Canyon Formation using Rietveld refined peak profiles, weakly shocked calcite from the crater rim appears to be indistinguishable from the tectonically deformed calcite. In contrast, Rietveld analysis readily distinguishes shocked Sierra Madera dolomite from unshocked equivalent dolostone samples from outside the crater and tectonically deformed Mission Canyon Formation dolomite.

X-ray diffraction from flight muscle with a headless myosin mutation: implications for interpreting reflection patterns

PubMed Central

Iwamoto, Hiroyuki; Trombitás, Károly; Yagi, Naoto; Suggs, Jennifer A.; Bernstein, Sanford I.

2014-01-01

Fruit fly (Drosophila melanogaster) is one of the most useful animal models to study the causes and effects of hereditary diseases because of its rich genetic resources. It is especially suitable for studying myopathies caused by myosin mutations, because specific mutations can be induced to the flight muscle-specific myosin isoform, while leaving other isoforms intact. Here we describe an X-ray-diffraction-based method to evaluate the structural effects of mutations in contractile proteins in Drosophila indirect flight muscle. Specifically, we describe the effect of the headless myosin mutation, Mhc10-Y97, in which the motor domain of the myosin head is deleted, on the X-ray diffraction pattern. The loss of general integrity of the filament lattice is evident from the pattern. A striking observation, however, is the prominent meridional reflection at d = 14.5 nm, a hallmark for the regularity of the myosin-containing thick filament. This reflection has long been considered to arise mainly from the myosin head, but taking the 6th actin layer line reflection as an internal control, the 14.5-nm reflection is even stronger than that of wild-type muscle. We confirmed these results via electron microscopy, wherein image analysis revealed structures with a similar periodicity. These observations have major implications on the interpretation of myosin-based reflections. PMID:25400584

Predicting the performance of airborne antennas in the microwave regime

NASA Astrophysics Data System (ADS)

Carroll, David P.

1990-12-01

This study investigated the application of a high-frequency model (Uniform Geometrical Theory of Diffraction) of electromagnetic sources mounted on a curved surface of a complex structure. In particular, the purpose of the study was to determine if the model could be used to predict the radiation patterns of cavity-backed spiral antennas mounted on aircraft fuselages so that the optimum locations for the antennas could be chosen during the aircraft design phase. A review of literature revealed a good deal of work in modeling communications, navigation, identification antennas (blade monopoles and aperture slots) mounted on a wide variety of aircraft fuselages and successful validation against quarter-scale model measurements. This study developed a monopole-array model of a spiral antenna's radiation at vertical polarization and an ellipsoid-plate model of the FB-111A. Using the antenna and aircraft models, the existing Uniform Geometrical Theory of Diffraction model generated radiation patterns which agreed favorably with full-scale measured data. The study includes plots of predicted and measured radiation patterns from 2.5 to 15 Gigahertz.

Ultrathin Cr added Ru film as a seedless Cu diffusion barrier for advanced Cu interconnects

NASA Astrophysics Data System (ADS)

Hsu, Kuo-Chung; Perng, Dung-Ching; Yeh, Jia-Bin; Wang, Yi-Chun

2012-07-01

A 5 nm thick Cr added Ru film has been extensively investigated as a seedless Cu diffusion barrier. High-resolution transmission electron microscopy micrograph, X-ray diffraction (XRD) pattern and Fourier transform-electron diffraction pattern reveal that a Cr contained Ru (RuCr) film has a glassy microstructure and is an amorphous-like film. XRD patterns and sheet resistance data show that the RuCr film is stable up to 650 °C, which is approximately a 200 °C improvement in thermal stability as compared to that of the pure Ru film. X-ray photoelectron spectroscopy depth profiles show that the RuCr film can successfully block Cu diffusion, even after a 30-min 650 °C annealing. The leakage current of the Cu/5 nm RuCr/porous SiOCH/Si stacked structure is about two orders of magnitude lower than that of a pristine Ru sample for electric field below 1 MV/cm. The RuCr film can be a promising Cu diffusion barrier for advanced Cu metallization.

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

Computer-based classification of bacteria species by analysis of their colonies Fresnel diffraction patterns

NASA Astrophysics Data System (ADS)

Suchwalko, Agnieszka; Buzalewicz, Igor; Podbielska, Halina

2012-01-01

In the presented paper the optical system with converging spherical wave illumination for classification of bacteria species, is proposed. It allows for compression of the observation space, observation of Fresnel patterns, diffraction pattern scaling and low level of optical aberrations, which are not possessed by other optical configurations. Obtained experimental results have shown that colonies of specific bacteria species generate unique diffraction signatures. Analysis of Fresnel diffraction patterns of bacteria colonies can be fast and reliable method for classification and recognition of bacteria species. To determine the unique features of bacteria colonies diffraction patterns the image processing analysis was proposed. Classification can be performed by analyzing the spatial structure of diffraction patterns, which can be characterized by set of concentric rings. The characteristics of such rings depends on the bacteria species. In the paper, the influence of basic features and ring partitioning number on the bacteria classification, is analyzed. It is demonstrated that Fresnel patterns can be used for classification of following species: Salmonella enteritidis, Staplyococcus aureus, Proteus mirabilis and Citrobacter freundii. Image processing is performed by free ImageJ software, for which a special macro with human interaction, was written. LDA classification, CV method, ANOVA and PCA visualizations preceded by image data extraction were conducted using the free software R.

Structural and electron diffraction scaling of twisted graphene bilayers

NASA Astrophysics Data System (ADS)

Zhang, Kuan; Tadmor, Ellad B.

2018-03-01

Multiscale simulations are used to study the structural relaxation in twisted graphene bilayers and the associated electron diffraction patterns. The initial twist forms an incommensurate moiré pattern that relaxes to a commensurate microstructure comprised of a repeating pattern of alternating low-energy AB and BA domains surrounding a high-energy AA domain. The simulations show that the relaxation mechanism involves a localized rotation and shrinking of the AA domains that scales in two regimes with the imposed twist. For small twisting angles, the localized rotation tends to a constant; for large twist, the rotation scales linearly with it. This behavior is tied to the inverse scaling of the moiré pattern size with twist angle and is explained theoretically using a linear elasticity model. The results are validated experimentally through a simulated electron diffraction analysis of the relaxed structures. A complex electron diffraction pattern involving the appearance of weak satellite peaks is predicted for the small twist regime. This new diffraction pattern is explained using an analytical model in which the relaxation kinematics are described as an exponentially-decaying (Gaussian) rotation field centered on the AA domains. Both the angle-dependent scaling and diffraction patterns are in quantitative agreement with experimental observations. A Matlab program for extracting the Gaussian model parameters accompanies this paper.

Computer Simulation of Diffraction Patterns.

ERIC Educational Resources Information Center

Dodd, N. A.

1983-01-01

Describes an Apple computer program (listing available from author) which simulates Fraunhofer and Fresnel diffraction using vector addition techniques (vector chaining) and allows user to experiment with different shaped multiple apertures. Graphics output include vector resultants, phase difference, diffraction patterns, and the Cornu spiral…

Quantitative analysis of crystalline pharmaceuticals in tablets by pattern-fitting procedure using X-ray diffraction pattern.

PubMed

Takehira, Rieko; Momose, Yasunori; Yamamura, Shigeo

2010-10-15

A pattern-fitting procedure using an X-ray diffraction pattern was applied to the quantitative analysis of binary system of crystalline pharmaceuticals in tablets. Orthorhombic crystals of isoniazid (INH) and mannitol (MAN) were used for the analysis. Tablets were prepared under various compression pressures using a direct compression method with various compositions of INH and MAN. Assuming that X-ray diffraction pattern of INH-MAN system consists of diffraction intensities from respective crystals, observed diffraction intensities were fitted to analytic expression based on X-ray diffraction theory and separated into two intensities from INH and MAN crystals by a nonlinear least-squares procedure. After separation, the contents of INH were determined by using the optimized normalization constants for INH and MAN. The correction parameter including all the factors that are beyond experimental control was required for quantitative analysis without calibration curve. The pattern-fitting procedure made it possible to determine crystalline phases in the range of 10-90% (w/w) of the INH contents. Further, certain characteristics of the crystals in the tablets, such as the preferred orientation, size of crystallite, and lattice disorder were determined simultaneously. This method can be adopted to analyze compounds whose crystal structures are known. It is a potentially powerful tool for the quantitative phase analysis and characterization of crystals in tablets and powders using X-ray diffraction patterns. Copyright 2010 Elsevier B.V. All rights reserved.

Design of a variable-line-spacing grating pattern for spectrometers based on a grating Fresnel device.

PubMed

Li, Xinghui; Zhang, Jinchao; Zhou, Qian; Ni, Kai; Pang, Jinchao; Tian, Rui

2016-04-01

In this Letter, we propose a variable-line-spacing (VLS) grating pattern for a hybrid diffractive device termed a grating Fresnel (G-Fresnel) lens, which is used in spectrometers to improve spectral resolution over a wide spectral range. The VLS grating pattern disperses light of specific wavelengths with a different angle and position such that the aberration caused by the Fresnel surface can be compensated for. In this manner, high resolution can be achieved over a relatively wide spectral range. The VLS grating pattern is designed based on the least wave-change principle and simulated by ZEMAX. Results reveal that the VLS G-Fresnel device allows a subnanometer resolution over a spectral range of 200 nm.

Crystal structure determination of new antimitotic agent bis(p-fluorobenzyl)trisulfide.

PubMed

An, Haoyun; Hu, Xiurong; Gu, Jianming; Chen, Linshen; Xu, Weiming; Mo, Xiaopeng; Xu, Wanhong; Wang, Xiaobo; Xu, Xiao

2008-01-01

The purpose of this research was to investigate the physical characteristics and crystalline structure of bis(p-fluorobenzyl)trisulfide, a new anti-tumor agent. Methods used included X-ray single crystal diffraction, X-ray powder diffraction (XRPD), Fourier-transform infrared (FT-IR) spectroscopy, differential scanning calorimetric (DSC) and thermogravimetric (TG) analyses. The findings obtained with X-ray single crystal diffraction showed that a monoclinic unit cell was a = 12.266(1) A, b = 4.7757(4) A, c = 25.510(1) A, beta = 104.25(1) degrees ; cell volume = 1,448.4(2) A(3), Z = 4, and space group C2/c. The XRPD studies of the four crystalline samples, obtained by recrystallization from four different solvents, indicated that they had the same diffraction patterns. The diffraction pattern stimulated from the crystal structure data is in excellent agreement with the experimental results. In addition, the identical FT-IR spectra of the four crystalline samples revealed absorption bands corresponding to S-S and C-S stretching as well as the characteristic aromatic substitution. Five percent weight loss at 163.3 degrees C was observed when TG was used to study the decomposition process in the temperature range of 20-200 degrees C. DSC also allowed for the determination of onset temperatures at 60.4(1)-60.7(3) degrees C and peak temperatures at 62.1(3)-62.4(3) degrees C for the four crystalline samples studied. The results verified that the single crystal structure shared the same crystal form with the four crystalline samples investigated.

Electron-beam-irradiation-induced crystallization of amorphous solid phase change materials

NASA Astrophysics Data System (ADS)

Zhou, Dong; Wu, Liangcai; Wen, Lin; Ma, Liya; Zhang, Xingyao; Li, Yudong; Guo, Qi; Song, Zhitang

2018-04-01

The electron-beam-irradiation-induced crystallization of phase change materials in a nano sized area was studied by in situ transmission electron microscopy and selected area electron diffraction. Amorphous phase change materials changed to a polycrystalline state after being irradiated with a 200 kV electron beam for a long time. The results indicate that the crystallization temperature strongly depends on the difference in the heteronuclear bond enthalpy of the phase change materials. The selected area electron diffraction patterns reveal that Ge2Sb2Te5 is a nucleation-dominated material, when Si2Sb2Te3 and Ti0.5Sb2Te3 are growth-dominated materials.

Big Sky and Greenhorn Drill Holes and CheMin X-ray Diffraction

NASA Image and Video Library

2015-12-17

The graph at right presents information from the NASA Curiosity Mars rover's onboard analysis of rock powder drilled from the "Big Sky" and "Greenhorn" target locations, shown at left. X-ray diffraction analysis of the Greenhorn sample inside the rover's Chemistry and Mineralogy (CheMin) instrument revealed an abundance of silica in the form of noncrystalline opal. The broad hump in the background of the X-ray diffraction pattern for Greenhorn, compared to Big Sky, is diagnostic of opal. The image of Big Sky at upper left was taken by the rover's Mars Hand Lens Imager (MAHLI) camera the day the hole was drilled, Sept. 29, 2015, during the mission's 1,119th Martian day, or sol. The Greenhorn hole was drilled, and the MAHLI image at lower left was taken, on Oct. 18, 2015 (Sol 1137). http://photojournal.jpl.nasa.gov/catalog/PIA20272

CROSS-DISCIPLINARY PHYSICS AND RELATED AREAS OF SCIENCE AND TECHNOLOGY: The effect of substrate on magnetic properties of Co/Cu multilayer nanowire arrays

NASA Astrophysics Data System (ADS)

Ren, Yong; Wang, Jian-Bo; Liu, Qing-Fang; Han, Xiang-Hua; Xue, De-Sheng

2009-08-01

Ordered Co/Cu multilayer nanowire arrays have been fabricated into anodic aluminium oxide templates with Ag and Cu substrate by direct current electrodeposition. This paper studies the morphology, structure and magnetic properties by transmission electron microscopy, selective area electron diffraction, x-ray diffraction, and vibrating sample magnetometer. X-ray diffraction patterns reveal that both as-deposited nanowire arrays films exhibit face-centred cubic structure. Magnetic measurements indicate that the easy magnetization direction of Co/Cu multilayer nanowire arrays films on Ag substrate is perpendicular to the long axis of nanowire, whereas the easy magnetization direction of the sample with Cu substrate is parallel to the long axis of nanowire. The change of easy magnetization direction attributed to different substrates, and the magnetic properties of the nanowire arrays are discussed.

Efficient modeling of Bragg coherent x-ray nanobeam diffraction

DOE PAGES

Hruszkewycz, S. O.; Holt, M. V.; Allain, M.; ...

2015-07-02

X-ray Bragg diffraction experiments that utilize tightly focused coherent beams produce complicated Bragg diffraction patterns that depend on scattering geometry, characteristics of the sample, and properties of the x-ray focusing optic. In this paper, we use a Fourier-transform-based method of modeling the 2D intensity distribution of a Bragg peak and apply it to the case of thin films illuminated with a Fresnel zone plate in three different Bragg scattering geometries. Finally, the calculations agree well with experimental coherent diffraction patterns, demonstrating that nanodiffraction patterns can be modeled at nonsymmetric Bragg conditions with this approach—a capability critical for advancing nanofocused x-raymore » diffraction microscopy.« less

Holographic Reconstruction of Photoelectron Diffraction and Its Circular Dichroism for Local Structure Probing

NASA Astrophysics Data System (ADS)

Matsui, Fumihiko; Matsushita, Tomohiro; Daimon, Hiroshi

2018-06-01

The local atomic structure around a specific element atom can be recorded as a photoelectron diffraction pattern. Forward focusing peaks and diffraction rings around them indicate the directions and distances from the photoelectron emitting atom to the surrounding atoms. The state-of-the-art holography reconstruction algorithm enables us to image the local atomic arrangement around the excited atom in a real space. By using circularly polarized light as an excitation source, the angular momentum transfer from the light to the photoelectron induces parallax shifts in these diffraction patterns. As a result, stereographic images of atomic arrangements are obtained. These diffraction patterns can be used as atomic-site-resolved probes for local electronic structure investigation in combination with spectroscopy techniques. Direct three-dimensional atomic structure visualization and site-specific electronic property analysis methods are reviewed. Furthermore, circular dichroism was also found in valence photoelectron and Auger electron diffraction patterns. The investigation of these new phenomena provides hints for the development of new techniques for local structure probing.

Diffractive optical devices produced by light-assisted trapping of nanoparticles.

PubMed

Muñoz-Martínez, J F; Jubera, M; Matarrubia, J; García-Cabañes, A; Agulló-López, F; Carrascosa, M

2016-01-15

One- and two-dimensional diffractive optical devices have been fabricated by light-assisted trapping and patterning of nanoparticles. The method is based on the dielectrophoretic forces appearing in the vicinity of a photovoltaic crystal, such as Fe:LiNbO3, during or after illumination. By illumination with the appropriate light distribution, the nanoparticles are organized along patterns designed at will. One- and two-dimensional diffractive components have been achieved on X- and Z-cut Fe:LiNbO3 crystals, with their polar axes parallel and perpendicular to the crystal surface, respectively. Diffraction gratings with periods down to around a few micrometers have been produced using metal (Al, Ag) nanoparticles with radii in the range of 70-100 nm. Moreover, several 2D devices, such as Fresnel zone plates, have been also produced showing the potential of the method. The diffractive particle patterns remain stable when light is removed. A method to transfer the diffractive patterns to other nonphotovoltaic substrates, such as silica glass, has been also reported.

Resolution enhancement by extrapolation of coherent diffraction images: a quantitative study on the limits and a numerical study of nonbinary and phase objects.

PubMed

Latychevskaia, T; Chushkin, Y; Fink, H-W

2016-10-01

In coherent diffractive imaging, the resolution of the reconstructed object is limited by the numerical aperture of the experimental setup. We present here a theoretical and numerical study for achieving super-resolution by postextrapolation of coherent diffraction images, such as diffraction patterns or holograms. We demonstrate that a diffraction pattern can unambiguously be extrapolated from only a fraction of the entire pattern and that the ratio of the extrapolated signal to the originally available signal is linearly proportional to the oversampling ratio. Although there could be in principle other methods to achieve extrapolation, we devote our discussion to employing iterative phase retrieval methods and demonstrate their limits. We present two numerical studies; namely, the extrapolation of diffraction patterns of nonbinary and that of phase objects together with a discussion of the optimal extrapolation procedure. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Farbrication of diffractive optical elements on a Si chip by an imprint lithography using nonsymmetrical silicon mold

NASA Astrophysics Data System (ADS)

Hirai, Yoshihiko; Okano, Masato; Okuno, Takayuki; Toyota, Hiroshi; Yotsuya, Tsutomu; Kikuta, Hisao; Tanaka, Yoshio

2001-11-01

Fabrication of a fine diffractive optical element on a Si chip is demonstrated using imprint lithography. A chirped diffraction grating, which has modulated pitched pattern with curved cross section is fabricated by an electron beam lithography, where the exposure dose profile is automatically optimized by computer aided system. Using the resist pattern as an etching mask, anisotropic dry etching is performed to transfer the resist pattern profile to the Si chip. The etched Si substrate is used as a mold in the imprint lithography. The Si mold is pressed to a thin polymer (poly methyl methacrylate) on a Si chip. After releasing the mold, a fine diffractive optical pattern is successfully transferred to the thin polymer. This method is exceedingly useful for fabrication of integrated diffractive optical elements with electric circuits on a Si chip.

Diffraction of V-point singularities through triangular apertures.

PubMed

Ram, B S Bhargava; Sharma, Anurag; Senthilkumaran, P

2017-05-01

In this paper we present experimental studies on diffraction of V-point singularities through equilateral and isosceles right triangular apertures. When V-point index, also called Poincare-Hopf index (η), of the optical field is +1, the diffraction disintegrates it into two monstars/lemons. When V-point index η is -1, diffraction produces two stars. The diffraction pattern, unlike phase singularity, is insensitive to polarity of the polarization singularity and the intensity pattern remains invariant. Higher order V-point singularities are generated using Sagnac interferometer and it is observed that the diffraction disintegrates them into lower order C-points.

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.

Laser fresnel distance measuring system and method

NASA Technical Reports Server (NTRS)

Campbell, Jonathan W. (Inventor); Lehner, David L. (Inventor); Smalley, Larry L. (Inventor); Smith, legal representative, Molly C. (Inventor); Sanders, Alvin J. (Inventor); Earl, Dennis Duncan (Inventor); Allison, Stephen W. (Inventor); Smith, Kelly L. (Inventor)

2008-01-01

A method and system for determining range to a target are provided. A beam of electromagnetic energy is transmitted through an aperture in an opaque screen such that a portion of the beam passes through the aperture to generate a region of diffraction that varies as a function of distance from the aperture. An imaging system is focused on a target plane in the region of diffraction with the generated image being compared to known diffraction patterns. Each known diffraction pattern has a unique value associated therewith that is indicative of a distance from the aperture. A match between the generated image and at least one of the known diffraction patterns is indicative of a distance between the aperture and target plane.

Phase Compositions of Self Reinforcement Al2O3/CaAl12O19 Composite using X-ray Diffraction Data and Rietveld Technique

NASA Astrophysics Data System (ADS)

Asmi, D.; Low, I. M.; O'Connor, B.

2008-03-01

The analysis of x-ray diffraction (XRD) patterns by the Rietveld technique was tested to the quantitatively phase compositions of self reinforcement Al2O3/CaAl12O19 composite. Room-temperature XRD patterns revealed that α-Al2O3 was the only phase presence in the CA0 sample, whereas the α-Al2O3 and CaAl12O19 phases were found for CA5, CA15, CA30, and CA50 samples. The peak intensity of CA6 in the self reinforcement Al2O3/CaAl12O19 composites increased in proportion with increase in CaAl12O19 content in contrast to α-Al2O3. The diffraction patterns for CA100 sample shows minor traces of α-Al2O3 even in relatively low peak intensity. It is suggesting that the in-situ reaction sintering of raw materials were not react completely to form 100 wt% CaAl12O19 at temperature 1650 °C. Quantitative phase compositions of self reinforcement Al2O3/CaAl12O19 composites by Rietveld analysis with XRD data has been well demonstrated. The results showed that the GOF values are relatively low and the fluctuation in the difference plots shows a reasonable fit between the observed and the calculated plot.

Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

Chongad, L. S.; Sharma, A.; Banerjee, M.; Jain, A.

2016-10-01

Lead sulfide (PbS) nanoparticles were prepared by chemical precipitation method (CPM) with the assistance of H2S gas. The microstructure and morphology of the synthesized nanoparticles have been investigated using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the PbS nanoparticles reveal formation of cubic phase. To investigate the quality of prepared nanoparticles, the particles size, lattice constant, strain, dislocation density etc. have been determined using XRD. TEM images reveal formation of cubic nanoparticles and the particle size determined from TEM images agree well with those from XRD.

Cryptotomography: reconstructing 3D Fourier intensities from randomly oriented single-shot diffraction patterns (CXIDB ID 9)

DOE Data Explorer

Loh, Ne-Te Duane

2011-08-01

These 2000 single-shot diffraction patterns include were either background-scattering only or hits (background-scattering plus diffraction signal from sub-micron ellipsoidal particles at random, undetermined orientations). Candidate hits were identified by eye, and the remainder were presumed as background. 54 usable, background-subtracted hits in this set (procedure in referenced article) were used to reconstruct the 3D diffraction intensities of the average ellipsoidal particle.

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

Optical diffraction properties of multimicrogratings

DOE PAGES

Rothenbach, Christian A.; Kravchenko, Ivan I.; Gupta, Mool C.

2015-02-27

This paper shows the results of optical diffraction properties of multimicrograting structures fabricated by e-beam lithography. Multimicrograting consist of arrays of hexagonally shaped cells containing periodic one-dimensional (1D) grating lines in different orientations and arrayed to form large area patterns. We analyzed the optical diffraction properties of multimicrogratings by studying the individual effects of the several periodic elements of multimicrogratings. The observed optical diffraction pattern is shown to be the combined effect of the periodic and non-periodic elements that define the multimicrogratings and the interaction between different elements. We measured the total transverse electric (TE) diffraction efficiency of multimicrogratings andmore » found it to be 32.1%, which is closely related to the diffraction efficiency of 1D periodic grating lines of the same characteristics, measured to be 33.7%. Beam profiles of the optical diffraction patterns from multimicrogratings are captured with a CCD sensor technique. Interference fringes were observed under certain conditions formed by multimicrograting beams interfering with each other. Finally, these diffraction structures may find applications in sensing, nanometrology, and optical interconnects.« less

Structural, morphological, optical and electrical properties of Schottky diodes based on CBD deposited ZnO:Cu nanorods

NASA Astrophysics Data System (ADS)

Mwankemwa, Benard S.; Legodi, Matshisa J.; Mlambo, Mbuso; Nel, Jackie M.; Diale, Mmantsae

2017-07-01

Undoped and copper doped zinc oxide (ZnO) nanorods have been synthesized by a simple chemical bath deposition (CBD) method at a temperature of 90 °C. Structural, morphological, optical and electrical properties of the synthesized ZnO nanorods were found to be dependent on the Cu doping percentage. X-ray diffraction (XRD) patterns revealed strong diffraction peaks of hexagonal wurtzite of ZnO, and no impurity phases from metallic zinc or copper. Scanning electron microscopy (SEM) images showed changes in diameter and shape of nanorods, where by those doped with 2 at.% and 3 at.% aggregated and became compact. Selected area electron diffraction (SAED) patterns indicates high quality, single crystalline wurtzite structure ZnO and intensities of bright spots varied with copper doping concentration. UV-visible absorption peaks of ZnO red shifted with increasing copper doping concentration. Raman studies demonstrated among others, strong and sharp E2 (low) and E2 (high) optical phonon peaks confirming crystal structure of ZnO. Current-voltage measurements based on the gold/ZnO nanorods/ITO showed good rectifying behavior of the Schottky diode. The predicted Schottky barrier height of 0.60 eV was obtained which is not far from the theoretical Schottky-Mott value of 0.80 eV.

Structure and giant magnetoresistance of granular Co-Cu nanolayers prepared by cross-beam pulsed laser deposition

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

Jesche, A.; Stoecker, H.; Levin, A. A.

2010-01-15

A series of Co{sub x}Cu{sub 100-x} (x=0, 40-75, 100) layers with thicknesses between 13 and 55 nm were prepared on silicon substrates using cross-beam pulsed laser deposition. Wide-angle x-ray diffraction (WAXRD), transmission electron microscopy (TEM), and electrical transport measurements revealed a structure consisting of decomposed cobalt and copper grains with grain sizes of about 10 nm. The influence of cobalt content and layer thickness on the grain size is discussed. Electron diffraction indicates the presence of an intermetallic Co-Cu phase of Cu{sub 3}Au structure type. Thermal treatment at temperatures between 525 and 750 K results in the progressive decomposition ofmore » Co and Cu, with an increase of the grain sizes up to about 100 nm. This is tunable by controlling the temperature and duration of the anneal, and is directly observable in WAXRD patterns and TEM images. A careful analysis of grain size and the coherence length of the radiation used allows for an accurate interpretation of the x-ray diffraction patterns, by taking into account coherent and noncoherent scattering. The alloy films show a giant magnetoresistance of 1%-2.3% with the maximum obtained after annealing at around 725 K.« less

Optical-diffraction method for determining crystal orientation

DOEpatents

Sopori, B.L.

1982-05-07

Disclosed is an optical diffraction technique for characterizing the three-dimensional orientation of a crystal sample. An arbitrary surface of the crystal sample is texture etched so as to generate a pseudo-periodic diffraction grating on the surface. A laser light beam is then directed onto the etched surface, and the reflected light forms a farfield diffraction pattern in reflection. Parameters of the diffraction pattern, such as the geometry and angular dispersion of the diffracted beam are then related to grating shape of the etched surface which is in turn related to crystal orientation. This technique may be used for examining polycrystalline silicon for use in solar cells.

Diffraction pattern simulation of cellulose fibrils using distributed and quantized pair distances

DOE PAGES

Zhang, Yan; Inouye, Hideyo; Crowley, Michael; ...

2016-10-14

Intensity simulation of X-ray scattering from large twisted cellulose molecular fibrils is important in understanding the impact of chemical or physical treatments on structural properties such as twisting or coiling. This paper describes a highly efficient method for the simulation of X-ray diffraction patterns from complex fibrils using atom-type-specific pair-distance quantization. Pair distances are sorted into arrays which are labelled by atom type. Histograms of pair distances in each array are computed and binned and the resulting population distributions are used to represent the whole pair-distance data set. These quantized pair-distance arrays are used with a modified and vectorized Debyemore » formula to simulate diffraction patterns. This approach utilizes fewer pair distances in each iteration, and atomic scattering factors are moved outside the iteration since the arrays are labelled by atom type. As a result, this algorithm significantly reduces the computation time while maintaining the accuracy of diffraction pattern simulation, making possible the simulation of diffraction patterns from large twisted fibrils in a relatively short period of time, as is required for model testing and refinement.« less

Diffraction pattern simulation of cellulose fibrils using distributed and quantized pair distances

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

Zhang, Yan; Inouye, Hideyo; Crowley, Michael

Intensity simulation of X-ray scattering from large twisted cellulose molecular fibrils is important in understanding the impact of chemical or physical treatments on structural properties such as twisting or coiling. This paper describes a highly efficient method for the simulation of X-ray diffraction patterns from complex fibrils using atom-type-specific pair-distance quantization. Pair distances are sorted into arrays which are labelled by atom type. Histograms of pair distances in each array are computed and binned and the resulting population distributions are used to represent the whole pair-distance data set. These quantized pair-distance arrays are used with a modified and vectorized Debyemore » formula to simulate diffraction patterns. This approach utilizes fewer pair distances in each iteration, and atomic scattering factors are moved outside the iteration since the arrays are labelled by atom type. This algorithm significantly reduces the computation time while maintaining the accuracy of diffraction pattern simulation, making possible the simulation of diffraction patterns from large twisted fibrils in a relatively short period of time, as is required for model testing and refinement.« less

Diffraction pattern simulation of cellulose fibrils using distributed and quantized pair distances

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

Zhang, Yan; Inouye, Hideyo; Crowley, Michael

Intensity simulation of X-ray scattering from large twisted cellulose molecular fibrils is important in understanding the impact of chemical or physical treatments on structural properties such as twisting or coiling. This paper describes a highly efficient method for the simulation of X-ray diffraction patterns from complex fibrils using atom-type-specific pair-distance quantization. Pair distances are sorted into arrays which are labelled by atom type. Histograms of pair distances in each array are computed and binned and the resulting population distributions are used to represent the whole pair-distance data set. These quantized pair-distance arrays are used with a modified and vectorized Debyemore » formula to simulate diffraction patterns. This approach utilizes fewer pair distances in each iteration, and atomic scattering factors are moved outside the iteration since the arrays are labelled by atom type. As a result, this algorithm significantly reduces the computation time while maintaining the accuracy of diffraction pattern simulation, making possible the simulation of diffraction patterns from large twisted fibrils in a relatively short period of time, as is required for model testing and refinement.« less

Non-spectroscopic composition measurements of SrTiO 3-La 0.7Sr 0.3MnO 3 multilayers using scanning convergent beam electron diffraction

DOE PAGES

Ophus, Colin; Ercius, Peter; Huijben, Mark; ...

2017-02-08

The local atomic structure of a crystalline sample aligned along a zone axis can be probed with a focused electron probe, which produces a convergent beam electron diffraction pattern. The introduction of high speed direct electron detectors has allowed for experiments that can record a full diffraction pattern image at thousands of probe positions on a sample. By incoherently summing these patterns over crystalline unit cells, we demonstrate in this paper that in addition to crystal structure and thickness, we can also estimate the local composition of a perovskite superlattice sample. This is achieved by matching the summed patterns tomore » a library of simulated diffraction patterns. Finally, this technique allows for atomic-scale chemical measurements without requiring a spectrometer or hardware aberration correction.« less

Transparent Electrochemical Gratings from a Patterned Bistable Silver Mirror.

PubMed

Park, Chihyun; Na, Jongbeom; Han, Minsu; Kim, Eunkyoung

2017-07-25

Silver mirror patterns were formed reversibly on a polystyrene (PS)-patterned electrode to produce gratings through the electrochemical reduction of silver ions. The electrochemical gratings exhibited high transparency (T > 95%), similar to a see-through window, by matching the refractive index of the grating pattern with the surrounding medium. The gratings switch to a diffractive state upon the formation of a mirror pattern (T < 5%) with a high diffraction efficiency up to 40%, providing reversible diffractive gratings. The diffraction state was maintained in the voltage-off state (V-off) for 40 min, which demonstrated bistable reversible electrochemical grating (BREG) behavior. By carefully combining the BREGs through period matching, dual-color switching was achieved within the full color region, which exhibited three distinct optical switching states between -2.5, 0, and +2.5 V. The wide range of light tenability using the metallic BREGs developed herein enabled IR modulation, NIR light reflection, and on-demand heat transfer.

Near-field diffraction from amplitude diffraction gratings: theory, simulation and results

NASA Astrophysics Data System (ADS)

Abedin, Kazi Monowar; Rahman, S. M. Mujibur

2017-08-01

We describe a computer simulation method by which the complete near-field diffract pattern of an amplitude diffraction grating can be generated. The technique uses the method of iterative Fresnel integrals to calculate and generate the diffraction images. Theoretical background as well as the techniques to perform the simulation is described. The program is written in MATLAB, and can be implemented in any ordinary PC. Examples of simulated diffraction images are presented and discussed. The generated images in the far-field where they reduce to Fraunhofer diffraction pattern are also presented for a realistic grating, and compared with the results predicted by the grating equation, which is applicable in the far-field. The method can be used as a tool to teach the complex phenomenon of diffraction in classrooms.

Micropatterned 2D Hybrid Perovskite Thin Films with Enhanced Photoluminescence Lifetimes.

PubMed

Kamminga, Machteld E; Fang, Hong-Hua; Loi, Maria Antonietta; Ten Brink, Gert H; Blake, Graeme R; Palstra, Thomas T M; Ten Elshof, Johan E

2018-04-18

The application of luminescent materials in display screens and devices requires micropatterned structures. In this work, we have successfully printed microstructures of a two-dimensional (2D), orange-colored organic/inorganic hybrid perovskite ((C 6 H 5 CH 2 NH 3 ) 2 PbI 4 ) using two different soft lithography techniques. Notably, both techniques yield microstructures with very high aspect ratios in the range of 1.5-1.8. X-ray diffraction reveals a strong preferential orientation of the crystallites along the c-axis in both patterned structures, when compared to nonpatterned, drop-casted thin films. Furthermore, (time-resolved) photoluminescence (PL) measurements reveal that the optical properties of (C 6 H 5 CH 2 NH 3 ) 2 PbI 4 are conserved upon patterning. We find that the larger grain sizes of the patterned films with respect to the nonpatterned film give rise to an enhanced PL lifetime. Thus, our results demonstrate easy and cost-effective ways to manufacture patterns of 2D organic/inorganic hybrid perovskites, while even improving their optical properties. This demonstrates the potential use of color-tunable 2D hybrids in optoelectronic devices.

Non-Destructive Quantification of Plastic Deformation in Steel: Employing X-Ray Diffraction Peak Broadening Analysis

DTIC Science & Technology

2013-09-01

pattern of an alloy, such as steel , reveals, among other properties (ex., phase composition, crystal structure), information about the strain state...This, together with elastic strain / residual stress analysis, would enable better evaluation of the current state of health of steel structures and...plastic strain in a component/structure may better evaluate the current state of health of steel structures and components as they near predetermined

Calculation of Debye-Scherrer diffraction patterns from highly stressed polycrystalline materials

DOE PAGES

MacDonald, M. J.; Vorberger, J.; Gamboa, E. J.; ...

2016-06-07

Calculations of Debye-Scherrer diffraction patterns from polycrystalline materials have typically been done in the limit of small deviatoric stresses. Although these methods are well suited for experiments conducted near hydrostatic conditions, more robust models are required to diagnose the large strain anisotropies present in dynamic compression experiments. A method to predict Debye-Scherrer diffraction patterns for arbitrary strains has been presented in the Voigt (iso-strain) limit. Here, we present a method to calculate Debye-Scherrer diffraction patterns from highly stressed polycrystalline samples in the Reuss (iso-stress) limit. This analysis uses elastic constants to calculate lattice strains for all initial crystallite orientations, enablingmore » elastic anisotropy and sample texture effects to be modeled directly. Furthermore, the effects of probing geometry, deviatoric stresses, and sample texture are demonstrated and compared to Voigt limit predictions. An example of shock-compressed polycrystalline diamond is presented to illustrate how this model can be applied and demonstrates the importance of including material strength when interpreting diffraction in dynamic compression experiments.« less

Sucrose lyophiles: a semi-quantitative study of residual water content by total X-ray diffraction analysis.

PubMed

Bates, S; Jonaitis, D; Nail, S

2013-10-01

Total X-ray Powder Diffraction Analysis (TXRPD) using transmission geometry was able to observe significant variance in measured powder patterns for sucrose lyophilizates with differing residual water contents. Integrated diffraction intensity corresponding to the observed variances was found to be linearly correlated to residual water content as measured by an independent technique. The observed variance was concentrated in two distinct regions of the lyophilizate powder pattern, corresponding to the characteristic sucrose matrix double halo and the high angle diffuse region normally associated with free-water. Full pattern fitting of the lyophilizate powder patterns suggested that the high angle variance was better described by the characteristic diffraction profile of a concentrated sucrose/water system rather than by the free-water diffraction profile. This suggests that the residual water in the sucrose lyophilizates is intimately mixed at the molecular level with sucrose molecules forming a liquid/solid solution. The bound nature of the residual water and its impact on the sucrose matrix gives an enhanced diffraction response between 3.0 and 3.5 beyond that expected for free-water. The enhanced diffraction response allows semi-quantitative analysis of residual water contents within the studied sucrose lyophilizates to levels below 1% by weight. Copyright © 2013 Elsevier B.V. All rights reserved.

Diffractive shear interferometry for extreme ultraviolet high-resolution lensless imaging

NASA Astrophysics Data System (ADS)

Jansen, G. S. M.; de Beurs, A.; Liu, X.; Eikema, K. S. E.; Witte, S.

2018-05-01

We demonstrate a novel imaging approach and associated reconstruction algorithm for far-field coherent diffractive imaging, based on the measurement of a pair of laterally sheared diffraction patterns. The differential phase profile retrieved from such a measurement leads to improved reconstruction accuracy, increased robustness against noise, and faster convergence compared to traditional coherent diffractive imaging methods. We measure laterally sheared diffraction patterns using Fourier-transform spectroscopy with two phase-locked pulse pairs from a high harmonic source. Using this approach, we demonstrate spectrally resolved imaging at extreme ultraviolet wavelengths between 28 and 35 nm.

Growth, structure, and magnetic properties of γ-Fe2O3 epitaxial films on MgO

NASA Astrophysics Data System (ADS)

Gao, Y.; Kim, Y. J.; Thevuthasan, S.; Chambers, S. A.; Lubitz, P.

1997-04-01

Single-crystal epitaxial thin films of γ-Fe2O3(001) have been grown on MgO(001) using oxygen-plasma-assisted molecular beam epitaxy. The structure and magnetic properties of these films have been characterized by a variety of techniques, including reflection high-energy electron diffraction (RHEED), low-energy electron diffraction (LEED), x-ray photoelectron spectroscopy and x-ray photoelectron/Auger electron diffraction (XPD/AED), vibrating sample magnetometry, and ferromagnetic resonance. Real-time RHEED reveals that the film growth occurs in a layer-by-layer fashion. The γ-Fe2O3(001) film surface exhibits a (1×1) LEED pattern. The growth of γ-Fe2Ooverflow="scroll">3 films at 450 °C is accompanied by significant Mg outdiffusion. AED of Mg KLL Auger emission reveals that Mg substitutionally incorporates in the γ-Fe2O3 lattice, occupying the octahedral sites. Magnetic moments are ˜2300 G and ˜4500 G for γ-Fe2O3 films grown at 250 °C and 450 °C, respectively. The high magnetic moment for the films grown at 450 °C could be attributed to the high degree of structural order of the films and Mg substitution at octahedral sites.

Quadrupole radiation from terahertz dipole antennas.

PubMed

Rudd, J V; Johnson, J L; Mittleman, D M

2000-10-15

We report what is to our knowledge the first detailed investigation of the polarization state of radiation from lens-coupled terahertz dipole antennas. The radiation exhibits a weak but measurable component that is polarized orthogonally to the orientation of the emitter dipole. The angular radiation pattern of this cross-polarized emission reveals that it is quadrupolar, rather than dipolar, in nature. One can understand this result by taking into account the photocurrent flowing in the strip lines that feed the dipole antenna. A Fresnel-Kirchhoff scalar diffraction calculation is used for calculating the frequency-dependent angular distribution of the radiation pattern, providing satisfactory agreement with the measurements.

Densely packed beta-structure at the protein-lipid interface of porin is revealed by high-resolution cryo-electron microscopy.

PubMed

Sass, H J; Büldt, G; Beckmann, E; Zemlin, F; van Heel, M; Zeitler, E; Rosenbusch, J P; Dorset, D L; Massalski, A

1989-09-05

Porin is an integral membrane protein that forms channels across the outer membrane of Escherichia coli. Electron microscopic studies of negatively stained two-dimensional porin crystals have shown three stain accumulations per porin trimer, revealing the locations of pores spanning the membrane. In this study, reconstituted porin lattices embedded in glucose were investigated using the low-dose technique on a cryo-electron microscope equipped with a helium-cooled superconducting objective lens. The specimen temperature was maintained at 5 K to yield an improved microscopic and specimen stability. Under these conditions, we obtained for the first time electron diffraction patterns from porin lattices to a resolution of 3.2 A and images showing optical diffraction up to a resolution of 4.9 A. Applying correlation averaging techniques to the digitized micrographs, we were able to reconstruct projected images of the porin trimer to a resolution of up to 3.5 A. In the final projection maps, amplitudes from electron diffraction and phases from these images were combined. The predominant feature is a high-density narrow band (about 6 A in thickness) that delineates the outer perimeter of the trimer. Since the molecule consists of almost exclusively beta-sheet structure, as revealed by spectroscopic data, we conclude that this band is a cylindrical beta-pleated sheet crossing the membrane nearly perpendicularly to its plane. Another intriguing finding is a low-density area (about 70 A2) situated in the centre of the trimer.

Local terahertz field enhancement for time-resolved x-ray diffraction

DOE PAGES

Kozina, M.; Pancaldi, M.; Bernhard, C.; ...

2017-02-20

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Local terahertz field enhancement for time-resolved x-ray diffraction

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

Kozina, M.; Pancaldi, M.; Bernhard, C.

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Rosalind Franklin's X-ray photo of DNA as an undergraduate optical diffraction experiment

NASA Astrophysics Data System (ADS)

Thompson, J.; Braun, G.; Tierney, D.; Wessels, L.; Schmitzer, H.; Rossa, B.; Wagner, H. P.; Dultz, W.

2018-02-01

Rosalind Franklin's X-ray diffraction patterns of DNA molecules rendered the important clue that DNA has the structure of a double helix. The most famous X-ray photograph, Photo 51, is still printed in most Biology textbooks. We suggest two optical experiments for undergraduates that make this historic achievement comprehensible for students by using macromodels of DNA and visible light to recreate a diffraction pattern similar to Photo 51. In these macromodels, we replace the double helix both mathematically and experimentally with its two-dimensional (flat) projection and explain why this is permissible. Basic optical concepts are used to infer certain well-known characteristics of DNA from the diffraction pattern.

High quality single shot diffraction patterns using ultrashort megaelectron volt electron beams from a radio frequency photoinjector.

PubMed

Musumeci, P; Moody, J T; Scoby, C M; Gutierrez, M S; Bender, H A; Wilcox, N S

2010-01-01

Single shot diffraction patterns using a 250-fs-long electron beam have been obtained at the UCLA Pegasus laboratory. High quality images with spatial resolution sufficient to distinguish closely spaced peaks in the Debye-Scherrer ring pattern have been recorded by scattering the 1.6 pC 3.5 MeV electron beam generated in the rf photoinjector off a 100-nm-thick Au foil. Dark current and high emittance particles are removed from the beam before sending it onto the diffraction target using a 1 mm diameter collimating hole. These results open the door to the study of irreversible phase transformations by single shot MeV electron diffraction.

Analysis of XFEL serial diffraction data from individual crystalline fibrils

PubMed Central

Wojtas, David H.; Ayyer, Kartik; Liang, Mengning; Mossou, Estelle; Romoli, Filippo; Seuring, Carolin; Beyerlein, Kenneth R.; Bean, Richard J.; Morgan, Andrew J.; Oberthuer, Dominik; Fleckenstein, Holger; Heymann, Michael; Gati, Cornelius; Yefanov, Oleksandr; Barthelmess, Miriam; Ornithopoulou, Eirini; Galli, Lorenzo; Xavier, P. Lourdu; Ling, Wai Li; Frank, Matthias; Yoon, Chun Hong; White, Thomas A.; Bajt, Saša; Mitraki, Anna; Boutet, Sebastien; Aquila, Andrew; Barty, Anton; Forsyth, V. Trevor; Chapman, Henry N.; Millane, Rick P.

2017-01-01

Serial diffraction data collected at the Linac Coherent Light Source from crystalline amyloid fibrils delivered in a liquid jet show that the fibrils are well oriented in the jet. At low fibril concentrations, diffraction patterns are recorded from single fibrils; these patterns are weak and contain only a few reflections. Methods are developed for determining the orientation of patterns in reciprocal space and merging them in three dimensions. This allows the individual structure amplitudes to be calculated, thus overcoming the limitations of orientation and cylindrical averaging in conventional fibre diffraction analysis. The advantages of this technique should allow structural studies of fibrous systems in biology that are inaccessible using existing techniques. PMID:29123682

Coherent diffraction imaging analysis of shape-controlled nanoparticles with focused hard X-ray free-electron laser pulses.

PubMed

Takahashi, Yukio; Suzuki, Akihiro; Zettsu, Nobuyuki; Oroguchi, Tomotaka; Takayama, Yuki; Sekiguchi, Yuki; Kobayashi, Amane; Yamamoto, Masaki; Nakasako, Masayoshi

2013-01-01

We report the first demonstration of the coherent diffraction imaging analysis of nanoparticles using focused hard X-ray free-electron laser pulses, allowing us to analyze the size distribution of particles as well as the electron density projection of individual particles. We measured 1000 single-shot coherent X-ray diffraction patterns of shape-controlled Ag nanocubes and Au/Ag nanoboxes and estimated the edge length from the speckle size of the coherent diffraction patterns. We then reconstructed the two-dimensional electron density projection with sub-10 nm resolution from selected coherent diffraction patterns. This method enables the simultaneous analysis of the size distribution of synthesized nanoparticles and the structures of particles at nanoscale resolution to address correlations between individual structures of components and the statistical properties in heterogeneous systems such as nanoparticles and cells.

NOTE: Calculating diffraction patterns

NASA Astrophysics Data System (ADS)

Rioux, Frank

2003-05-01

Following Marcella's approach to the double-slit experiment (Marcella T V 2002 Eur. J. Phys. 23 615-21), diffraction patterns for two-dimensional masks are calculated by Fourier transform of the Mask geometry into momentum space.

Robust reconstruction of time-resolved diffraction from ultrafast streak cameras

PubMed Central

Badali, Daniel S.; Dwayne Miller, R. J.

2017-01-01

In conjunction with ultrafast diffraction, streak cameras offer an unprecedented opportunity for recording an entire molecular movie with a single probe pulse. This is an attractive alternative to conventional pump-probe experiments and opens the door to studying irreversible dynamics. However, due to the “smearing” of the diffraction pattern across the detector, the streaking technique has thus far been limited to simple mono-crystalline samples and extreme care has been taken to avoid overlapping diffraction spots. In this article, this limitation is addressed by developing a general theory of streaking of time-dependent diffraction patterns. Understanding the underlying physics of this process leads to the development of an algorithm based on Bayesian analysis to reconstruct the time evolution of the two-dimensional diffraction pattern from a single streaked image. It is demonstrated that this approach works on diffraction peaks that overlap when streaked, which not only removes the necessity of carefully choosing the streaking direction but also extends the streaking technique to be able to study polycrystalline samples and materials with complex crystalline structures. Furthermore, it is shown that the conventional analysis of streaked diffraction can lead to erroneous interpretations of the data. PMID:28653022

Diffraction-based BioCD biosensor for point-of-care diagnostics

NASA Astrophysics Data System (ADS)

Choi, H.; Chang, C.; Savran, C.; Nolte, D.

2018-02-01

The BioCD platform technology uses spinning-disk interferometry to detect molecular binding to target molecular probes in biological samples. Interferometric configurations have included differential phase contrast and in-line quadrature detection. For the detection of extremely low analyte concentrations, nano- or microparticles can enhance the signal through background-free diffraction detection. Diffraction signal measurements on BioCD biosensors are achieved by forming gratings on a disc surface. The grating pattern was printed with biotinylated bovine serum albumin (BSA) and streptavidin coated beads were deployed. The diameter of the beads was 1 micron and strong protein bonding occurs between BSA and streptavidin-coated beads at the printed location. The wavelength for the protein binding detection was 635 nm. The periodic pattern on the disc amplified scattered light into the first-order diffraction position. The diffracted signal contains Mie scattering and a randomly-distributed-bead noise contributions. Variation of the grating pattern periodicity modulates the diffraction efficiency. To test multiple spatial frequencies within a single scan, we designed a fan-shaped grating to perform frequency filter multiplexing on a diffraction-based BioCD.

Nanometres-resolution Kikuchi patterns from materials science specimens with transmission electron forward scatter diffraction in the scanning electron microscope.

PubMed

Brodusch, N; Demers, H; Gauvin, R

2013-04-01

A charge-coupled device camera of an electron backscattered diffraction system in a scanning electron microscope was positioned below a thin specimen and transmission Kikuchi patterns were collected. Contrary to electron backscattered diffraction, transmission electron forward scatter diffraction provides phase identification and orientation mapping at the nanoscale. The minimum Pd particle size for which a Kikuchi diffraction pattern was detected and indexed reliably was 5.6 nm. An orientation mapping resolution of 5 nm was measured at 30 kV. The resolution obtained with transmission electron forward scatter diffraction was of the same order of magnitude than that reported in electron nanodiffraction in the transmission electron microscope. An energy dispersive spectrometer X-ray map and a transmission electron forward scatter diffraction orientation map were acquired simultaneously. The high-resolution chemical, phase and orientation maps provided at once information on the chemical form, orientation and coherency of precipitates in an aluminium-lithium 2099 alloy. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Research on Near Field Pattern Effects.

DTIC Science & Technology

1981-01-01

block numbr) High frequency solutions Prolate spheroid mounted antennas Uniform Geometrical Theory of Diffraction Airborne antenna pattern predicti...Geometrical Theory of Diffraction solutions which were developed previously were DD 1473 EDITION OF I NOV 66 IS OBSOLETE UCASFE SECURITY CLASSIFICATION...be used later to simulate the fuselage of a general aircraft. The general uniform Geometrical Theory of Diffraction (GTD) solutions [1i which are

Ptychographic overlap constraint errors and the limits of their numerical recovery using conjugate gradient descent methods.

PubMed

Tripathi, Ashish; McNulty, Ian; Shpyrko, Oleg G

2014-01-27

Ptychographic coherent x-ray diffractive imaging is a form of scanning microscopy that does not require optics to image a sample. A series of scanned coherent diffraction patterns recorded from multiple overlapping illuminated regions on the sample are inverted numerically to retrieve its image. The technique recovers the phase lost by detecting the diffraction patterns by using experimentally known constraints, in this case the measured diffraction intensities and the assumed scan positions on the sample. The spatial resolution of the recovered image of the sample is limited by the angular extent over which the diffraction patterns are recorded and how well these constraints are known. Here, we explore how reconstruction quality degrades with uncertainties in the scan positions. We show experimentally that large errors in the assumed scan positions on the sample can be numerically determined and corrected using conjugate gradient descent methods. We also explore in simulations the limits, based on the signal to noise of the diffraction patterns and amount of overlap between adjacent scan positions, of just how large these errors can be and still be rendered tractable by this method.

Optical diffraction for measurements of nano-mechanical bending

NASA Astrophysics Data System (ADS)

Hermans, Rodolfo I.; Dueck, Benjamin; Ndieyira, Joseph Wafula; McKendry, Rachel A.; Aeppli, Gabriel

2016-06-01

We explore and exploit diffraction effects that have been previously neglected when modelling optical measurement techniques for the bending of micro-mechanical transducers such as cantilevers for atomic force microscopy. The illumination of a cantilever edge causes an asymmetric diffraction pattern at the photo-detector affecting the calibration of the measured signal in the popular optical beam deflection technique (OBDT). The conditions that avoid such detection artefacts conflict with the use of smaller cantilevers. Embracing diffraction patterns as data yields a potent detection technique that decouples tilt and curvature and simultaneously relaxes the requirements on the illumination alignment and detector position through a measurable which is invariant to translation and rotation. We show analytical results, numerical simulations and physiologically relevant experimental data demonstrating the utility of the diffraction patterns. We offer experimental design guidelines and quantify possible sources of systematic error in OBDT. We demonstrate a new nanometre resolution detection method that can replace OBDT, where diffraction effects from finite sized or patterned cantilevers are exploited. Such effects are readily generalized to cantilever arrays, and allow transmission detection of mechanical curvature, enabling instrumentation with simpler geometry. We highlight the comparative advantages over OBDT by detecting molecular activity of antibiotic Vancomycin.

Synchrotron X-Ray Diffraction Studies of Olivine from Comet Wild 2

NASA Technical Reports Server (NTRS)

2008-01-01

We have analyzed a collection of the Comet Wild 2 coma grains returned by the NASA Stardust Mission, using micro-area Laue diffraction equipment. The purpose of the diffraction experiment is to permit the structure refinement of olivine including site occupancies. In addition to the intrinsic importance of the olivine structures for revealing the thermal history of Wild 2 materials, we wish to test reports that olivine recovered after hypervelocity capture in silica aerogel has undergone a basic structural change due to capture heating [1]. The diffraction equipment placed at beam line BL- 4B1 of PF, KEK was developed with a micropinhole and an imaging plate (Fuji Co. Ltd.) using the Laue method combined with polychromatic X-ray of synchrotron radiation operated at energy of 2.5 GeV. The incident beam is limited to 1.6 m in diameter by a micropinhole set just upstream of the sample [2, 3]. It is essential to apply a microbeam to obtain diffracted intensities with high signal to noise ratios. This equipment has been successfully applied to various extraterrestrial materials, including meteorites and interplanetary dust particles [4]. The Laue pattern of the sample C2067,1,111,4 (Fig. 1) was successfully taken on an imaging plate after a 120 minute exposure (Fig. 2).

Diffractive imaging of a rotational wavepacket in nitrogen molecules with femtosecond megaelectronvolt electron pulses

DOE PAGES

Yang, Jie; Guehr, Markus; Vecchione, Theodore; ...

2016-04-05

Imaging changes in molecular geometries on their natural femtosecond timescale with sub-Angström spatial precision is one of the critical challenges in the chemical sciences, as the nuclear geometry changes determine the molecular reactivity. For photoexcited molecules, the nuclear dynamics determine the photoenergy conversion path and efficiency. Here we report a gas-phase electron diffraction experiment using megaelectronvolt (MeV) electrons, where we captured the rotational wavepacket dynamics of nonadiabatically laser-aligned nitrogen molecules. We achieved a combination of 100 fs root-mean-squared temporal resolution and sub-Angstrom (0.76 Å) spatial resolution that makes it possible to resolve the position of the nuclei within the molecule.more » In addition, the diffraction patterns reveal the angular distribution of the molecules, which changes from prolate (aligned) to oblate (anti-aligned) in 300 fs. Lastly, our results demonstrate a significant and promising step towards making atomically resolved movies of molecular reactions.« less

A quantum diffractor for thermal flux

NASA Astrophysics Data System (ADS)

José Martínez-Pérez, Maria; Giazotto, Francesco

2014-04-01

Macroscopic phase coherence between weakly coupled superconductors leads to peculiar interference phenomena. Among these, magnetic flux-driven diffraction might be produced, in full analogy to light diffraction through a rectangular slit. This can be experimentally revealed by the electric current and, notably, also by the heat current transmitted through the circuit. The former was observed more than 50 years ago and represented the first experimental evidence of the phase-coherent nature of the Josephson effect, whereas the second one was still lacking. Here we demonstrate the existence of heat diffraction by measuring the modulation of the electronic temperature of a small metallic electrode nearby-contacted to a thermally biased short Josephson junction subjected to an in-plane magnetic field. The observed temperature dependence exhibits symmetry under magnetic flux reversal, and clear resemblance with a Fraunhofer-like modulation pattern. Our approach, joined to widespread methods for phase-biasing superconducting circuits, might represent an effective tool for controlling the thermal flux in nanoscale devices.

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.

Multiple Optical Traps with a Single-Beam Optical Tweezer Utilizing Surface Micromachined Planar Curved Grating

NASA Astrophysics Data System (ADS)

Kuo, Ju-Nan; Chen, Kuan-Yu

2010-11-01

In this paper, we present a single-beam optical tweezer integrated with a planar curved diffraction grating for microbead manipulation. Various curvatures of the surface micromachined planar curved grating are systematically investigated. The planar curved grating was fabricated using multiuser micro-electro-mechanical-system (MEMS) processes (MUMPs). The angular separation and the number of diffracted orders were determined. Experimental results indicate that the diffraction patterns and curvature of the planar curved grating are closely related. As the curvature of the planar curved grating increases, the vertical diffraction angle increases, resulting in the strip patterns of the planar curved grating. A single-beam optical tweezer integrated with a planar curved diffraction grating was developed. We demonstrate a technique for creating multiple optical traps from a single laser beam using the developed planar curved grating. The strip patterns of the planar curved grating that resulted from diffraction were used to trap one row of polystyrene beads.

Computer Simulation Of An In-Process Surface Finish Sensor.

NASA Astrophysics Data System (ADS)

Rakels, Jan H.

1987-01-01

It is generally accepted, that optical methods are the most promising for the in-process measurement of surface finish. These methods have the advantages of being non-contacting and fast data acquisition. Furthermore, these optical instruments can be easily retrofitted on existing machine-tools. In the Micro-Engineering Centre at the University of Warwick, an optical sensor has been developed which can measure the rms roughness, slope and wavelength of turned and precision ground surfaces during machining. The operation of this device is based upon the Kirchhoff-Fresnel diffraction integral. Application of this theory to ideal turned and ground surfaces is straightforward, and indeed the calculated diffraction patterns are in close agreement with patterns produced by an actual optical instrument. Since it is mathematically difficult to introduce real machine-tool behaviour into the diffraction integral, a computer program has been devised, which simulates the operation of the optical sensor. The program produces a diffraction pattern as a graphical output. Comparison between computer generated and actual diffraction patterns of the same surfaces show a high correlation. The main aim of this program is to construct an atlas, which maps known machine-tool errors versus optical diffraction patterns. This atlas can then be used for machine-tool condition diagnostics. It has been found that optical monitoring is very sensitive to minor defects. Therefore machine-tool detoriation can be detected before it is detrimental.

Two-photon x-ray diffraction

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

Stohr, J.

The interference pattern of a circular photon source has long been used to define the optical diffraction limit. Here we show the breakdown of conventional x-ray diffraction theory for the fundamental case of a “source”, consisting of a back-illuminated thin film in a circular aperture. When the conventional spontaneous x-ray scattering by atoms in the film is replaced at high incident intensity by stimulated resonant scattering, the film becomes the source of cloned photon twins and the diffraction pattern becomes self-focused beyond the diffraction limit. Furthermore, the case of cloned photon pairs is compared to and distinguished from entangled photonmore » pairs or biphotons.« less

Two-photon x-ray diffraction

DOE PAGES

Stohr, J.

2017-01-11

The interference pattern of a circular photon source has long been used to define the optical diffraction limit. Here we show the breakdown of conventional x-ray diffraction theory for the fundamental case of a “source”, consisting of a back-illuminated thin film in a circular aperture. When the conventional spontaneous x-ray scattering by atoms in the film is replaced at high incident intensity by stimulated resonant scattering, the film becomes the source of cloned photon twins and the diffraction pattern becomes self-focused beyond the diffraction limit. Furthermore, the case of cloned photon pairs is compared to and distinguished from entangled photonmore » pairs or biphotons.« less

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

PubMed

Tang, M X; Zhang, Y Y; E, J C; Luo, S N

2018-05-01

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

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

Tang, M. X.; Zhang, Y. Y.; E, J. C.

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of themore » diffraction patterns is discussed.« less

Three-dimensional electron diffraction of plant light-harvesting complex

PubMed Central

Wang, Da Neng; Kühlbrandt, Werner

1992-01-01

Electron diffraction patterns of two-dimensional crystals of light-harvesting chlorophyll a/b-protein complex (LHC-II) from photosynthetic membranes of pea chloroplasts, tilted at different angles up to 60°, were collected to 3.2 Å resolution at -125°C. The reflection intensities were merged into a three-dimensional data set. The Friedel R-factor and the merging R-factor were 21.8 and 27.6%, respectively. Specimen flatness and crystal size were critical for recording electron diffraction patterns from crystals at high tilts. The principal sources of experimental error were attributed to limitations of the number of unit cells contributing to an electron diffraction pattern, and to the critical electron dose. The distribution of strong diffraction spots indicated that the three-dimensional structure of LHC-II is less regular than that of other known membrane proteins and is not dominated by a particular feature of secondary structure. ImagesFIGURE 1FIGURE 2 PMID:19431817

Fabrication of Si3N4 thin films on phynox alloy substrates for electronic applications

NASA Astrophysics Data System (ADS)

Shankernath, V.; Naidu, K. Lakshun; Krishna, M. Ghanashyam; Padmanabhan, K. A.

2018-04-01

Thin films of Si3N4 are deposited on Phynox alloy substrates using radio frequency magnetron sputtering. The thickness of the films was varied between 80-150 nm by increasing the duration of deposition from 1 to 3 h at a fixed power density and working pressure. X-ray diffraction patterns reveal that the Si3N4 films had crystallized inspite of the substrates not being heated during deposition. This was confirmed using selected area electron diffraction and high resolution transmission electron microscopy also. It is postulated that a low lattice misfit between Si3N4 and Phynox provides energetically favourable conditions for ambient temperature crystallization. The hardness of the films is of the order of 6 to 9 GPa.

Synthesis and characterization of gold nanodogbones by the seeded mediated growth method

NASA Astrophysics Data System (ADS)

Huang, Chien-Jung; Chiu, Pin-Hsiang; Wang, Yeong-Her; Meen, Teen-Hang; Yang, Cheng-Fu

2007-10-01

Novel gold nanodogbones (GDBs) are successfully fabricated using a simple seeded mediated growth (SMG) method. The shapes of GDBs depend on the amount of added vitamin C solvent. The amount of vitamin C solvent was varied from 10 to 40 µl to investigate the influence of vitamin C solvent on the GDBs. It is found that the aspect ratios (R) of GDBs were in the range from 2.34 to 1.46, and the UV-vis absorption measurement revealed a pronounced blueshift on the longitudinal surface plasmon resonance (SPR) band from 713 to 676 nm. The GDBs were determined by x-ray diffraction (XRD) to be single-crystalline with a face-centered cubic (fcc) structure. The lattice constant calculated from this selected-area electron diffraction (SAED) pattern is 4.068 Å.

X-ray diffraction, FTIR, UV-VIS and SEM studies on chromium (III) complexes

NASA Astrophysics Data System (ADS)

Mishra, Ashutosh; Dwivedi, Jagrati; Shukla, Kritika

2015-06-01

Five Chromium (III) complexes have been prepared using Schiff base ligands which derived from benzoin and five different amino acids (H2N-R). Samples were characterized by XRD, FTIR, UV-VIS and SEM method. X-Ray diffraction pattern analyzed that all chromium (III) complexes have hexagonal structure and crystalline, in nature, using Bruker D8 Advance instrument. Using VERTAX 70, FTIR spectroscopy reveals that Samples have (C=N), (C-O), (M-N) and (M-O) bonds in the range of 4000-400cm-1. UV-VIS spectroscopy give information that samples absorb the visible light which is in the range of 380-780nm. For this, Lambda 960 spectrometer used. SEM is designed for studying of the solid objects, using JEOL JSM 5600 instrument.

Dark-field imaging based on post-processed electron backscatter diffraction patterns of bulk crystalline materials in a scanning electron microscope.

PubMed

Brodusch, Nicolas; Demers, Hendrix; Gauvin, Raynald

2015-01-01

Dark-field (DF) images were acquired in the scanning electron microscope with an offline procedure based on electron backscatter diffraction (EBSD) patterns (EBSPs). These EBSD-DF images were generated by selecting a particular reflection on the electron backscatter diffraction pattern and by reporting the intensity of one or several pixels around this point at each pixel of the EBSD-DF image. Unlike previous studies, the diffraction information of the sample is the basis of the final image contrast with a pixel scale resolution at the EBSP providing DF imaging in the scanning electron microscope. The offline facility of this technique permits the selection of any diffraction condition available in the diffraction pattern and displaying the corresponding image. The high number of diffraction-based images available allows a better monitoring of deformation structures compared to electron channeling contrast imaging (ECCI) which is generally limited to a few images of the same area. This technique was applied to steel and iron specimens and showed its high capability in describing more rigorously the deformation structures around micro-hardness indents. Due to the offline relation between the reference EBSP and the EBSD-DF images, this new technique will undoubtedly greatly improve our knowledge of deformation mechanism and help to improve our understanding of the ECCI contrast mechanisms. Copyright © 2014 Elsevier B.V. All rights reserved.

Analysis of XFEL serial diffraction data from individual crystalline fibrils

DOE PAGES

Wojtas, David H.; Ayyer, Kartik; Liang, Mengning; ...

2017-10-20

Serial diffraction data collected at the Linac Coherent Light Source from crystalline amyloid fibrils delivered in a liquid jet show that the fibrils are well oriented in the jet. At low fibril concentrations, diffraction patterns are recorded from single fibrils; these patterns are weak and contain only a few reflections. Methods are developed for determining the orientation of patterns in reciprocal space and merging them in three dimensions. This allows the individual structure amplitudes to be calculated, thus overcoming the limitations of orientation and cylindrical averaging in conventional fibre diffraction analysis. In conclusion, the advantages of this technique should allowmore » structural studies of fibrous systems in biology that are inaccessible using existing techniques.« less

Analysis of XFEL serial diffraction data from individual crystalline fibrils

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

Wojtas, David H.; Ayyer, Kartik; Liang, Mengning

Serial diffraction data collected at the Linac Coherent Light Source from crystalline amyloid fibrils delivered in a liquid jet show that the fibrils are well oriented in the jet. At low fibril concentrations, diffraction patterns are recorded from single fibrils; these patterns are weak and contain only a few reflections. Methods are developed for determining the orientation of patterns in reciprocal space and merging them in three dimensions. This allows the individual structure amplitudes to be calculated, thus overcoming the limitations of orientation and cylindrical averaging in conventional fibre diffraction analysis. In conclusion, the advantages of this technique should allowmore » structural studies of fibrous systems in biology that are inaccessible using existing techniques.« less

Observation of electromigration in a Cu thin line by in situ coherent x-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Takahashi, Yukio; Nishino, Yoshinori; Furukawa, Hayato; Kubo, Hideto; Yamauchi, Kazuto; Ishikawa, Tetsuya; Matsubara, Eiichiro

2009-06-01

Electromigration (EM) in a 1-μm-thick Cu thin line was investigated by in situ coherent x-ray diffraction microscopy (CXDM). Characteristic x-ray speckle patterns due to both EM-induced voids and thermal deformation in the thin line were observed in the coherent x-ray diffraction patterns. Both parts of the voids and the deformation were successfully visualized in the images reconstructed from the diffraction patterns. This result not only represents the first demonstration of the visualization of structural changes in metallic materials by in situ CXDM but is also an important step toward studying the structural dynamics of nanomaterials using x-ray free-electron lasers in the near future.

Electromagnetic scattering by impedance structures

NASA Technical Reports Server (NTRS)

Balanis, Constantine A.; Griesser, Timothy

1987-01-01

The scattering of electromagnetic waves from impedance structures is investigated, and current work on antenna pattern calculation is presented. A general algorithm for determining radiation patterns from antennas mounted near or on polygonal plates is presented. These plates are assumed to be of a material which satisfies the Leontovich (or surface impedance) boundary condition. Calculated patterns including reflection and diffraction terms are presented for numerious geometries, and refinements are included for antennas mounted directly on impedance surfaces. For the case of a monopole mounted on a surface impedance ground plane, computed patterns are compared with experimental measurements. This work in antenna pattern prediction forms the basis of understanding of the complex scattering mechanisms from impedance surfaces. It provides the foundation for the analysis of backscattering patterns which, in general, are more problematic than calculation of antenna patterns. Further proposed study of related topics, including surface waves, corner diffractions, and multiple diffractions, is outlined.

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

Calculation of Debye-Scherrer diffraction patterns from highly stressed polycrystalline materials

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

MacDonald, M. J., E-mail: macdonm@umich.edu; SLAC National Accelerator Laboratory, Menlo Park, California 94025; Vorberger, J.

2016-06-07

Calculations of Debye-Scherrer diffraction patterns from polycrystalline materials have typically been done in the limit of small deviatoric stresses. Although these methods are well suited for experiments conducted near hydrostatic conditions, more robust models are required to diagnose the large strain anisotropies present in dynamic compression experiments. A method to predict Debye-Scherrer diffraction patterns for arbitrary strains has been presented in the Voigt (iso-strain) limit [Higginbotham, J. Appl. Phys. 115, 174906 (2014)]. Here, we present a method to calculate Debye-Scherrer diffraction patterns from highly stressed polycrystalline samples in the Reuss (iso-stress) limit. This analysis uses elastic constants to calculate latticemore » strains for all initial crystallite orientations, enabling elastic anisotropy and sample texture effects to be modeled directly. The effects of probing geometry, deviatoric stresses, and sample texture are demonstrated and compared to Voigt limit predictions. An example of shock-compressed polycrystalline diamond is presented to illustrate how this model can be applied and demonstrates the importance of including material strength when interpreting diffraction in dynamic compression experiments.« less

Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2016-07-06

Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

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

Latychevskaia, Tatiana, E-mail: tatiana@physik.uzh.ch; Fink, Hans-Werner; Chushkin, Yuriy

Coherent diffraction imaging is a high-resolution imaging technique whose potential can be greatly enhanced by applying the extrapolation method presented here. We demonstrate the enhancement in resolution of a non-periodical object reconstructed from an experimental X-ray diffraction record which contains about 10% missing information, including the pixels in the center of the diffraction pattern. A diffraction pattern is extrapolated beyond the detector area and as a result, the object is reconstructed at an enhanced resolution and better agreement with experimental amplitudes is achieved. The optimal parameters for the iterative routine and the limits of the extrapolation procedure are discussed.

Study of thermal stability of spontaneously grown superlattice structures by metalorganic vapor phase epitaxy in AlxGa1-xAs/GaAs heterostructure

NASA Astrophysics Data System (ADS)

Pradhan, A.; Maitra, T.; Mukherjee, S.; Mukherjee, S.; Satpati, B.; Nayak, A.; Bhunia, S.

2018-04-01

Spontaneous superlattice ordering in a length scale larger than an atomic layer has been observed in AlxGa1-xAs layers grown on (100) GaAs substrates by metalorganic vapor phase epitaxy. Transmission electron microscopic image clearly revealed superlattice structures and the selected area electron diffraction showed closely spaced superlattice spots around the main diffraction pattern. High resolution x-ray diffraction showed distinct and sharp superlattice peaks symmetrically positioned around the central (004) Bragg peak and the similar measurement for (002) planes, which is quasi-forbidden for Bragg reflections showed only superlattice peaks. Thermal annealing studies showed the superlattice structure was stable up to 800 °C and disappeared after annealing at 900 °C retaining the crystallinity of the epilayer. Study of inter-diffusivitiesin such superlattice structures has been carried out using high temperaturex-ray diffraction results. Here we present (004) x-ray θ-2θ scans of the AlGaAs/GaAs (100) sample with annealing time for different temperatures. Conclusions regarding interdiffusion in such superlattice structures are drawn from high temperature X-ray measurements.

Hexamethylenetetramine assisted hydrothermal synthesis of BiPO4 and its electrochemical properties for supercapacitors

NASA Astrophysics Data System (ADS)

Nithya, V. D.; Kalai Selvan, R.; Vasylechko, Leonid

2015-11-01

The well defined microstructures of BiPO4 were successfully synthesized by the facile hexamethylenetetramine (HMT) assisted hydrothermal method. The low temperature monoclinic BiPO4 structure with space group P21/n, were obtained from X-ray diffraction (XRD) for the pristine and HMT-assisted BiPO4 with 1, 3, 5 and 10 mmole concentration. A transformation from low temperature monazite-type phase to the high temperature SbPO4-type phase of BiPO4 was observed at the 10 mmole concentration. There was a variation in the morphology from polyhedron to octahedra-like and finally into cube shape upon an increase in concentration of HMT. The role of reaction time in the morphology of BiPO4 particles was investigated. The selected area electron diffraction (SAED) pattern elucidated the ordered dot pattern and the calculated d-spacing revealed the formation of BiPO4. An increased specific capacitance of HMT assisted materials (202 F/g) compared with pristine BiPO4 (89 F/g) at 5 mA/cm2 was observed upon morphological variation due to HMT addition.

Crossover between Tilt Families and Zero Area Thermal Expansion in Hybrid Prussian Blue Analogues.

PubMed

Phillips, Anthony E; Fortes, A Dominic

2017-12-11

Materials in the family of Prussian blue analogues (C 3 H 5 N 2 ) 2 K[M(CN) 6 ], where C 3 H 5 N 2 is the imidazolium ion and M=Fe, Co, undergo two phase transitions with temperature; at low temperatures the imidazolium cations have an ordered configuration (C2/c), while in the intermediate- and high-temperature phases (both previously reported as R3‾m ) they are dynamically disordered. We show from high-resolution powder neutron diffraction data that the high-temperature phase has zero area thermal expansion in the ab-plane. Supported by Landau theory and single-crystal X-ray diffraction data, we re-evaluate the space group symmetry of the intermediate-temperature phase to R3‾ . This reveals that the low-to-intermediate temperature transition is due to competition between two different tilt patterns of the [M(CN) 6 ] 3- ions. Controlling the relative stabilities of these tilt patterns offers a potential means to tune the exploitable electric behaviour that arises from motion of the imidazolium guest. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Reflection high-energy electron diffraction measurements of reciprocal space structure of 2D materials.

PubMed

Xiang, Y; Guo, F-W; Lu, T-M; Wang, G-C

2016-12-02

Knowledge on the symmetry and perfection of a 2D material deposited or transferred to a surface is very important and valuable. We demonstrate a method to map the reciprocal space structure of 2D materials using reflection high energy diffraction (RHEED). RHEED from a 2D material gives rise to 'streaks' patterns. It is shown that from these streaks patterns at different azimuthal rotation angles that the reciprocal space intensity distribution can be constructed as a function of momentum transfer parallel to the surface. To illustrate the principle, we experimentally constructed the reciprocal space structure of a commercial graphene/SiO 2 /Si sample in which the graphene layer was transferred to the SiO 2 /Si substrate after it was deposited on a Cu foil by chemical vapor deposition. The result reveals a 12-fold symmetry of the graphene layer which is a result of two dominant orientation domains with 30° rotation relative to each other. We show that the graphene can serve as a template to grow other materials such as a SnS film that follows the symmetry of graphene.

Emergent Rotational Symmetries in Disordered Magnetic Domain Patterns

NASA Astrophysics Data System (ADS)

Su, Run; Seu, Keoki A.; Parks, Daniel; Kan, Jimmy J.; Fullerton, Eric E.; Roy, Sujoy; Kevan, Stephen D.

2011-12-01

Uniaxial systems often form labyrinthine domains that exhibit short-range order but are macroscopically isotropic and would not be expected to exhibit precise symmetries. However, their underlying frustration results in a multitude of metastable configurations of comparable energy, and driving such a system externally might lead to pattern formation. We find that soft x-ray speckle diffraction patterns of the labyrinthine domains in CoPd/IrMn heterostructures reveal a diverse array of hidden rotational symmetries about the magnetization axis, thereby suggesting an unusual form of emergent order in an otherwise disordered system. These symmetries depend on applied magnetic field, magnetization history, and scattering wave vector. Maps of rotational symmetry exhibit intriguing structures that can be controlled by manipulating the applied magnetic field in concert with the exchange bias condition.

Emergent rotational symmetries in disordered magnetic domain patterns.

PubMed

Su, Run; Seu, Keoki A; Parks, Daniel; Kan, Jimmy J; Fullerton, Eric E; Roy, Sujoy; Kevan, Stephen D

2011-12-16

Uniaxial systems often form labyrinthine domains that exhibit short-range order but are macroscopically isotropic and would not be expected to exhibit precise symmetries. However, their underlying frustration results in a multitude of metastable configurations of comparable energy, and driving such a system externally might lead to pattern formation. We find that soft x-ray speckle diffraction patterns of the labyrinthine domains in CoPd/IrMn heterostructures reveal a diverse array of hidden rotational symmetries about the magnetization axis, thereby suggesting an unusual form of emergent order in an otherwise disordered system. These symmetries depend on applied magnetic field, magnetization history, and scattering wave vector. Maps of rotational symmetry exhibit intriguing structures that can be controlled by manipulating the applied magnetic field in concert with the exchange bias condition. © 2011 American Physical Society

Calculating cellulose diffraction patterns

USDA-ARS?s Scientific Manuscript database

Although powder diffraction of cellulose is a common experiment, the patterns are not widely understood. The theory is mathematical, there are numerous different crystal forms, and the conventions are not standardized. Experience with IR spectroscopy is not directly transferable. An awful error, tha...

Publications - GMC 196 | Alaska Division of Geological & Geophysical

Science.gov Websites

DGGS GMC 196 Publication Details Title: X-ray diffraction patterns of clay from the following wells for more information. Bibliographic Reference Unknown, 1992, X-ray diffraction patterns of clay from

An investigation of phase transformation and crystallinity in laser surface modified H13 steel

NASA Astrophysics Data System (ADS)

Aqida, S. N.; Brabazon, D.; Naher, S.

2013-03-01

This paper presents a laser surface modification process of AISI H13 tool steel using 0.09, 0.2 and 0.4 mm size of laser spot with an aim to increase hardness properties. A Rofin DC-015 diffusion-cooled CO2 slab laser was used to process AISI H13 tool steel samples. Samples of 10 mm diameter were sectioned to 100 mm length in order to process a predefined circumferential area. The parameters selected for examination were laser peak power, overlap percentage and pulse repetition frequency (PRF). X-ray diffraction analysis (XRD) was conducted to measure crystallinity of the laser-modified surface. X-ray diffraction patterns of the samples were recorded using a Bruker D8 XRD system with Cu K α ( λ=1.5405 Å) radiation. The diffraction patterns were recorded in the 2 θ range of 20 to 80°. The hardness properties were tested at 981 mN force. The laser-modified surface exhibited reduced crystallinity compared to the un-processed samples. The presence of martensitic phase was detected in the samples processed using 0.4 mm spot size. Though there was reduced crystallinity, a high hardness was measured in the laser-modified surface. Hardness was increased more than 2.5 times compared to the as-received samples. These findings reveal the phase source of the hardening mechanism and grain composition in the laser-modified surface.

Reflector antennas with low sidelobes, low cross polarization, and high aperture efficiency

NASA Technical Reports Server (NTRS)

Faigen, I. M.; Reichert, C. F.; Sletten, C. J.; Shore, R. A.

1984-01-01

Techniques are presented for computing the horn near field patterns on the subreflectors and for correcting the phase center errors of the horn pattern by shaping the subreflector surface. The diffraction pattern computations for scanned beams are described. The effects of dish aperture diffraction on pattern bandwidth are investigated. A model antenna consisting of a reflector, shaped subreflector, and corrugated feed horn is described.

Importance of methodological standardization for the ektacytometric measures of red blood cell deformability in sickle cell anemia.

PubMed

Renoux, Céline; Parrow, Nermi; Faes, Camille; Joly, Philippe; Hardeman, Max; Tisdale, John; Levine, Mark; Garnier, Nathalie; Bertrand, Yves; Kebaili, Kamila; Cuzzubbo, Daniela; Cannas, Giovanna; Martin, Cyril; Connes, Philippe

2016-01-01

Red blood cell (RBC) deformability is severely decreased in patients with sickle cell anemia (SCA), which plays a role in the pathophysiology of the disease. However, investigation of RBC deformability from SCA patients demands careful methodological considerations. We assessed RBC deformability by ektacytometry (LORRCA MaxSis, Mechatronics, The Netherlands) in 6 healthy individuals and 49 SCA patients and tested the effects of different heights of the RBC diffraction patterns, obtained by altering the camera gain of the LORRCA, on the result of RBC deformability measurements, expressed as Elongation Index (EI). Results indicate that the pattern of RBCs from control subjects adopts an elliptical shape under shear stress, whereas the pattern of RBCs from individuals with SCA adopts a diamond shape arising from the superposition of elliptical and circular patterns. The latter represent rigid RBCs. While the EI measures did not change with the variations of the RBC diffraction pattern heights in the control subjects, we observed a decrease of EI when the RBC diffraction pattern height is increased in the SCA group. The differences in SCA EI values measured at 5 Pa between the different diffraction pattern heights correlated with the percent of hemoglobin S and the percent of sickled RBC observed by microscopy. Our study confirms that the camera gain or aperture of the ektacytometer should be used to standardize the size of the RBC diffraction pattern height when measuring RBC deformability in sickle cell patients and underscores the potential clinical utility of this technique.

A review and reassessment of diffraction, scattering, and shadows in electrodynamics

NASA Astrophysics Data System (ADS)

Berg, Matthew J.; Sorensen, Christopher M.

2018-05-01

The concepts of diffraction and scattering are well known and considered fundamental in optics and other wave phenomena. For any type of wave, one way to define diffraction is the spreading of waves, i.e., no change in the average propagation direction, while scattering is the deflection of waves with a clear change of propagation direction. However, the terms "diffraction" and "scattering" are often used interchangeably, and hence, a clear distinction between the two is difficult to find. This review considers electromagnetic waves and retains the simple definition that diffraction is the spreading of waves but demonstrates that all diffraction patterns are the result of scattering. It is shown that for electromagnetic waves, the "diffracted" wave from an object is the Ewald-Oseen extinction wave in the far-field zone. The intensity distribution of this wave yields what is commonly called the diffraction pattern. Moreover, this is the same Ewald-Oseen wave that cancels the incident wave inside the object and thereafter continues to do so immediately behind the object to create a shadow. If the object is much wider than the beam but has a hole, e.g., a screen with an aperture, the Ewald-Oseen extinction wave creates the shadow behind the screen and the incident light that passes through the aperture creates the diffraction pattern. This point of view also illustrates Babinet's principle. Thus, it is the Ewald-Oseen extinction theorem that binds together diffraction, scattering, and shadows.

Indexing amyloid peptide diffraction from serial femtosecond crystallography: new algorithms for sparse patterns

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

Brewster, Aaron S.; Sawaya, Michael R.; University of California, Los Angeles, CA 90095-1570

2015-02-01

Special methods are required to interpret sparse diffraction patterns collected from peptide crystals at X-ray free-electron lasers. Bragg spots can be indexed from composite-image powder rings, with crystal orientations then deduced from a very limited number of spot positions. Still diffraction patterns from peptide nanocrystals with small unit cells are challenging to index using conventional methods owing to the limited number of spots and the lack of crystal orientation information for individual images. New indexing algorithms have been developed as part of the Computational Crystallography Toolbox (cctbx) to overcome these challenges. Accurate unit-cell information derived from an aggregate data setmore » from thousands of diffraction patterns can be used to determine a crystal orientation matrix for individual images with as few as five reflections. These algorithms are potentially applicable not only to amyloid peptides but also to any set of diffraction patterns with sparse properties, such as low-resolution virus structures or high-throughput screening of still images captured by raster-scanning at synchrotron sources. As a proof of concept for this technique, successful integration of X-ray free-electron laser (XFEL) data to 2.5 Å resolution for the amyloid segment GNNQQNY from the Sup35 yeast prion is presented.« less

Dynamical scattering in coherent hard x-ray nanobeam Bragg diffraction

NASA Astrophysics Data System (ADS)

Pateras, A.; Park, J.; Ahn, Y.; Tilka, J. A.; Holt, M. V.; Kim, H.; Mawst, L. J.; Evans, P. G.

2018-06-01

Unique intensity features arising from dynamical diffraction arise in coherent x-ray nanobeam diffraction patterns of crystals having thicknesses larger than the x-ray extinction depth or exhibiting combinations of nanoscale and mesoscale features. We demonstrate that dynamical scattering effects can be accurately predicted using an optical model combined with the Darwin theory of dynamical x-ray diffraction. The model includes the highly divergent coherent x-ray nanobeams produced by Fresnel zone plate focusing optics and accounts for primary extinction, multiple scattering, and absorption. The simulation accurately reproduces the dynamical scattering features of experimental diffraction patterns acquired from a GaAs/AlGaAs epitaxial heterostructure on a GaAs (001) substrate.

Micropatterned 2D Hybrid Perovskite Thin Films with Enhanced Photoluminescence Lifetimes

PubMed Central

2018-01-01

The application of luminescent materials in display screens and devices requires micropatterned structures. In this work, we have successfully printed microstructures of a two-dimensional (2D), orange-colored organic/inorganic hybrid perovskite ((C6H5CH2NH3)2PbI4) using two different soft lithography techniques. Notably, both techniques yield microstructures with very high aspect ratios in the range of 1.5–1.8. X-ray diffraction reveals a strong preferential orientation of the crystallites along the c-axis in both patterned structures, when compared to nonpatterned, drop-casted thin films. Furthermore, (time-resolved) photoluminescence (PL) measurements reveal that the optical properties of (C6H5CH2NH3)2PbI4 are conserved upon patterning. We find that the larger grain sizes of the patterned films with respect to the nonpatterned film give rise to an enhanced PL lifetime. Thus, our results demonstrate easy and cost-effective ways to manufacture patterns of 2D organic/inorganic hybrid perovskites, while even improving their optical properties. This demonstrates the potential use of color-tunable 2D hybrids in optoelectronic devices. PMID:29578335

Meta-stable magnetic transitions and its field dependence in Co2.75Fe0.25O4 ferrite

NASA Astrophysics Data System (ADS)

Aswathi M., C.; Bhowmik, R. N.

2018-04-01

The Co2.75Fe0.25O4 ferrite has been prepared by chemical co-precipitation route. The as-prepared sample has been annealed at 500° C. X-ray diffraction pattern indicated cubic spinel structure in the sample. The sample showed ferrimagnetic nature with magnetic irreversibility and hysteresis loop. Magnetization data revealed high anisotropic nature and at least two prominent meta-stable magnetic transitions below the highest measurement temperature 350 K.

The measurement capabilities of cross-sectional profile of Nanoimprint template pattern using small angle x-ray scattering

NASA Astrophysics Data System (ADS)

Yamanaka, Eiji; Taniguchi, Rikiya; Itoh, Masamitsu; Omote, Kazuhiko; Ito, Yoshiyasu; Ogata, Kiyoshi; Hayashi, Naoya

2016-05-01

Nanoimprint lithography (NIL) is one of the most potential candidates for the next generation lithography for semiconductor. It will achieve the lithography with high resolution and low cost. High resolution of NIL will be determined by a high definition template. Nanoimprint lithography will faithfully transfer the pattern of NIL template to the wafer. Cross-sectional profile of the template pattern will greatly affect the resist profile on the wafer. Therefore, the management of the cross-sectional profile is essential. Grazing incidence small angle x-ray scattering (GI-SAXS) technique has been proposed as one of the method for measuring cross-sectional profile of periodic nanostructure pattern. Incident x-rays are irradiated to the sample surface with very low glancing angle. It is close to the critical angle of the total reflection of the x-ray. The scattered x-rays from the surface structure are detected on a two-dimensional detector. The observed intensity is discrete in the horizontal (2θ) direction. It is due to the periodicity of the structure, and diffraction is observed only when the diffraction condition is satisfied. In the vertical (β) direction, the diffraction intensity pattern shows interference fringes reflected to height and shape of the structure. Features of the measurement using x-ray are that the optical constant for the materials are well known, and it is possible to calculate a specific diffraction intensity pattern based on a certain model of the cross-sectional profile. The surface structure is estimated by to collate the calculated diffraction intensity pattern that sequentially while changing the model parameters with the measured diffraction intensity pattern. Furthermore, GI-SAXS technique can be measured an object in a non-destructive. It suggests the potential to be an effective tool for product quality assurance. We have developed a cross-sectional profile measurement of quartz template pattern using GI-SAXS technique. In this report, we will report the measurement capabilities of GI-SAXS technique as a cross-sectional profile measurement tool of NIL quartz template pattern.

Teaching Fraunhofer diffraction via experimental and simulated images in the laboratory

NASA Astrophysics Data System (ADS)

Peinado, Alba; Vidal, Josep; Escalera, Juan Carlos; Lizana, Angel; Campos, Juan; Yzuel, Maria

2012-10-01

Diffraction is an important phenomenon introduced to Physics university students in a subject of Fundamentals of Optics. In addition, in the Physics Degree syllabus of the Universitat Autònoma de Barcelona, there is an elective subject in Applied Optics. In this subject, diverse diffraction concepts are discussed in-depth from different points of view: theory, experiments in the laboratory and computing exercises. In this work, we have focused on the process of teaching Fraunhofer diffraction through laboratory training. Our approach involves students working in small groups. They visualize and acquire some important diffraction patterns with a CCD camera, such as those produced by a slit, a circular aperture or a grating. First, each group calibrates the CCD camera, that is to say, they obtain the relation between the distances in the diffraction plane in millimeters and in the computer screen in pixels. Afterwards, they measure the significant distances in the diffraction patterns and using the appropriate diffraction formalism, they calculate the size of the analyzed apertures. Concomitantly, students grasp the convolution theorem in the Fourier domain by analyzing the diffraction of 2-D gratings of elemental apertures. Finally, the learners use a specific software to simulate diffraction patterns of different apertures. They can control several parameters: shape, size and number of apertures, 1-D or 2-D gratings, wavelength, focal lens or pixel size.Therefore, the program allows them to reproduce the images obtained experimentally, and generate others by changingcertain parameters. This software has been created in our research group, and it is freely distributed to the students in order to help their learning of diffraction. We have observed that these hands on experiments help students to consolidate their theoretical knowledge of diffraction in a pedagogical and stimulating learning process.

Precession technique and electron diffractometry as new tools for crystal structure analysis and chemical bonding determination.

PubMed

Avilov, A; Kuligin, K; Nicolopoulos, S; Nickolskiy, M; Boulahya, K; Portillo, J; Lepeshov, G; Sobolev, B; Collette, J P; Martin, N; Robins, A C; Fischione, P

2007-01-01

We have developed a new fast electron diffractometer working with high dynamic range and linearity for crystal structure determinations. Electron diffraction (ED) patterns can be scanned serially in front of a Faraday cage detector; the total measurement time for several hundred ED reflections can be tens of seconds having high statistical accuracy for all measured intensities (1-2%). This new tool can be installed to any type of TEM without any column modification and is linked to a specially developed electron beam precession "Spinning Star" system. Precession of the electron beam (Vincent-Midgley technique) reduces dynamical effects allowing also use of accurate intensities for crystal structure analysis. We describe the technical characteristics of this new tool together with the first experimental results. Accurate measurement of electron diffraction intensities by electron diffractometer opens new possibilities not only for revealing unknown structures, but also for electrostatic potential determination and chemical bonding investigation. As an example, we present detailed atomic bonding information of CaF(2) as revealed for the first time by precise electron diffractometry.

X-Ray Diffraction of different samples of Swarna Makshika Bhasma.

PubMed

Gupta, Ramesh Kumar; Lakshmi, Vijay; Jha, Chandra Bhushan

2015-01-01

Shodhana and Marana are a series of complex procedures that identify the undesirable effects of heavy metals/minerals and convert them into absorbable and assimilable forms. Study on the analytical levels is essential to evaluate the structural and chemical changes that take place during and after following such procedures as described in major classical texts to understand the mystery behind these processes. X-Ray Diffraction (XRD) helps to identify and characterize minerals/metals and fix up the particular characteristics pattern of prepared Bhasma. To evaluate the chemical changes in Swarna Makshika Bhasma prepared by using different media and methods. In this study, raw Swarna Makshika, purified Swarna Makshika and four types of Swarna Makshika Bhasma prepared by using different media and methods were analyzed by XRD study. XRD study of different samples revealed strongest peaks of iron oxide in Bhasma. Other phases of Cu2O, FeS2, Cu2S, FeSO4, etc., were also identified in many of the samples. XRD study revealed that Swarna Makshika Bhasma prepared by Kupipakwa method is better, convenient, and can save time.

Excitation of phonons in medium-energy electron diffraction

NASA Astrophysics Data System (ADS)

Alvarez, M. A. Vicente; Ascolani, H.; Zampieri, G.

1996-03-01

The ``elastic'' backscattering of electrons from crystalline surfaces presents two regimes: a low-energy regime, in which the characteristic low-energy electron diffraction (LEED) pattern is observed, and a medium-energy regime, in which the diffraction pattern is similar to those observed in x-ray photoemission diffraction (XPD) and Auger electron diffraction (AED) experiments. We present a model for the electron scattering which, including the vibrational degrees of freedom of the crystal, contains both regimes and explains the passage from one regime to the other. Our model is based on a separation of the electron and atomic motions (adiabatic approximation) and on a cluster-type formulation of the multiple scattering of the electron. The inelastic scattering events (excitation and/or absorption of phonons) are treated as coherent processes and no break of the phase relation between the incident and the exit paths of the electron is assumed. The LEED and the medium-energy electron diffraction regimes appear naturally in this model as the limit cases of completely elastic scattering and of inelastic scattering with excitation and/or absorption of multiple phonons. Intensity patterns calculated with this model are in very good agreement with recent experiments of electron scattering on Cu(001) at low and medium energies. We show that there is a correspondence between the type of intensity pattern and the mean number of phonons excited and/or absorbed during the scattering: a LEED-like pattern is observed when this mean number is less than 2, LEED-like and XPD/AED-like features coexist when this number is 3-4, and a XPD/AED-like pattern is observed when this number is greater than 5-6.

A look inside epitaxial cobalt-on-fluorite nanoparticles with three-dimensional reciprocal space mapping using GIXD, RHEED and GISAXS.

PubMed

Suturin, S M; Fedorov, V V; Korovin, A M; Valkovskiy, G A; Konnikov, S G; Tabuchi, M; Sokolov, N S

2013-08-01

In this work epitaxial growth of cobalt on CaF 2 (111), (110) and (001) surfaces has been extensively studied. It has been shown by atomic force microscopy that at selected growth conditions stand-alone faceted Co nanoparticles are formed on a fluorite surface. Grazing-incidence X-ray diffraction (GIXD) and reflection high-energy electron diffraction (RHEED) studies have revealed that the particles crystallize in the face-centered cubic lattice structure otherwise non-achievable in bulk cobalt under normal conditions. The particles were found to inherit lattice orientation from the underlying CaF 2 layer. Three-dimensional reciprocal space mapping carried out using X-ray and electron diffraction has revealed that there exist long bright 〈111〉 streaks passing through the cobalt Bragg reflections. These streaks are attributed to stacking faults formed in the crystal lattice of larger islands upon coalescence of independently nucleated smaller islands. Distinguished from the stacking fault streaks, crystal truncation rods perpendicular to the {111} and {001} particle facets have been observed. Finally, grazing-incidence small-angle X-ray scattering (GISAXS) has been applied to decouple the shape-related scattering from that induced by the crystal lattice defects. Particle faceting has been verified by modeling the GISAXS patterns. The work demonstrates the importance of three-dimensional reciprocal space mapping in the study of epitaxial nanoparticles.

Growth, structure, and magnetic properties of {gamma}-Fe{sub 2}O{sub 3} epitaxial films on MgO

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

Gao, Y.; Kim, Y.J.; Thevuthasan, S.

1997-04-01

Single-crystal epitaxial thin films of {gamma}-Fe{sub 2}O{sub 3}(001) have been grown on MgO(001) using oxygen-plasma-assisted molecular beam epitaxy. The structure and magnetic properties of these films have been characterized by a variety of techniques, including reflection high-energy electron diffraction (RHEED), low-energy electron diffraction (LEED), x-ray photoelectron spectroscopy and x-ray photoelectron/Auger electron diffraction (XPD/AED), vibrating sample magnetometry, and ferromagnetic resonance. Real-time RHEED reveals that the film growth occurs in a layer-by-layer fashion. The {gamma}-Fe{sub 2}O{sub 3}(001) film surface exhibits a (1{times}1) LEED pattern. The growth of {gamma}-Fe{sub 2}O{sub 3} films at 450 {degree}C is accompanied by significant Mg outdiffusion. AED ofmore » Mg KLL Auger emission reveals that Mg substitutionally incorporates in the {gamma}-Fe{sub 2}O{sub 3} lattice, occupying the octahedral sites. Magnetic moments are {approximately}2300 G and {approximately}4500 G for {gamma}-Fe{sub 2}O{sub 3} films grown at 250{degree}C and 450{degree}C, respectively. The high magnetic moment for the films grown at 450{degree}C could be attributed to the high degree of structural order of the films and Mg substitution at octahedral sites. {copyright} {ital 1997 American Institute of Physics.}« less

A look inside epitaxial cobalt-on-fluorite nanoparticles with three-dimensional reciprocal space mapping using GIXD, RHEED and GISAXS

PubMed Central

Suturin, S. M.; Fedorov, V. V.; Korovin, A. M.; Valkovskiy, G. A.; Konnikov, S. G.; Tabuchi, M.; Sokolov, N. S.

2013-01-01

In this work epitaxial growth of cobalt on CaF2(111), (110) and (001) surfaces has been extensively studied. It has been shown by atomic force microscopy that at selected growth conditions stand-alone faceted Co nanoparticles are formed on a fluorite surface. Grazing-incidence X-ray diffraction (GIXD) and reflection high-energy electron diffraction (RHEED) studies have revealed that the particles crystallize in the face-centered cubic lattice structure otherwise non-achievable in bulk cobalt under normal conditions. The particles were found to inherit lattice orientation from the underlying CaF2 layer. Three-dimensional reciprocal space mapping carried out using X-ray and electron diffraction has revealed that there exist long bright 〈111〉 streaks passing through the cobalt Bragg reflections. These streaks are attributed to stacking faults formed in the crystal lattice of larger islands upon coalescence of independently nucleated smaller islands. Distinguished from the stacking fault streaks, crystal truncation rods perpendicular to the {111} and {001} particle facets have been observed. Finally, grazing-incidence small-angle X-ray scattering (GISAXS) has been applied to decouple the shape-related scattering from that induced by the crystal lattice defects. Particle faceting has been verified by modeling the GISAXS patterns. The work demonstrates the importance of three-dimensional reciprocal space mapping in the study of epitaxial nanoparticles. PMID:24046491

Shear induced weakening of the hydrogen bonding lattice of the energetic material 5,5'-Hydrazinebistetrazole at high-pressure

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

Ciezak-Jenkins, Jennifer A.; Jenkins, Timothy A.

5,5'-Hydrazinebistetrazole (HBTA) has been studied by in-situ x-ray diffraction and vibrational spectroscopy to pressures near 25 GPa at room temperature. Analysis of the x-ray diffraction pattern of HBTA collected at ambient pressure and temperature revealed a monoclinic structure consistent with that previously reported. Under compression, the x-ray diffraction reveals little evidence of a phase transition over the pressure range studied. Slight anisotropy in response to compression was noted and the β angle decreased moderately, suggesting geometry modifications occur in the hydrogen bonding lattice and between neighboring HBTA molecules as a result of compression along the c axis. Blue shifts inmore » the Infrared active N-H stretching modes were observed, implying a weakening of the hydrogen bond with compression. The weakening of the hydrogen bonding lattice with pressure may lead to an increase in the bending angle of the C-N=N-C bridge between the tetrazole rings and an increased overlap between the π-bonding orbitals. The Raman spectra showed a number of modes associated with H-N=N-H motions of the bridge become more prominent in the spectra under compression. Additionally, the possibility that the increased bend in the angle of the C-N=N-C bridge results from a shearing deformation is discussed.« less

Noniterative approach to the missing data problem in coherent diffraction imaging by phase retrieval.

PubMed

Nakajima, Nobuharu

2010-07-20

When a very intense beam is used for illuminating an object in coherent x-ray diffraction imaging, the intensities at the center of the diffraction pattern for the object are cut off by a beam stop that is utilized to block the intense beam. Until now, only iterative phase-retrieval methods have been applied to object reconstruction from a single diffraction pattern with a deficiency of central data due to a beam stop. As an alternative method, I present a noniterative solution in which an interpolation method based on the sampling theorem for the missing data is used for object reconstruction with our previously proposed phase-retrieval method using an aperture-array filter. Computer simulations demonstrate the reconstruction of a complex-amplitude object from a single diffraction pattern with a missing data area, which is generally difficult to treat with the iterative methods because a nonnegativity constraint cannot be used for such an object.

An E-plane analysis of aperture-matched horn antennas using the moment method and the uniform geometrical theory of diffraction

NASA Technical Reports Server (NTRS)

Heedy, D. J.; Burnside, W. D.

1984-01-01

The moment method and the uniform geometrical theory of diffraction are utilized to obtain two separate solutions for the E-plane field pattern of an aperture-matched horn antenna. This particular horn antenna consists of a standard pyramidal horn with the following modifications: a rolled edge section attached to the aperture edges and a curved throat section. The resulting geometry provides significantly better performance in terms of the pattern, impedance, and frequency characteristics than normally obtainable. The moment method is used to calculate the E-plane pattern and BSWR of the antenna. However, at higher frequencies, large amounts of computation time are required. The uniform geometrical theory of diffraction provides a quick and efficient high frequency solution for the E-plane field pattern. In fact, the uniform geometrical theory of diffraction may be used to initially design the antenna; then, the moment method may be applied to fine tune the design. This procedure has been successfully applied to a compact range feed design.

Indexing amyloid peptide diffraction from serial femtosecond crystallography: New algorithms for sparse patterns

DOE PAGES

Brewster, Aaron S.; Sawaya, Michael R.; Rodriguez, Jose; ...

2015-01-23

Still diffraction patterns from peptide nanocrystals with small unit cells are challenging to index using conventional methods owing to the limited number of spots and the lack of crystal orientation information for individual images. New indexing algorithms have been developed as part of the Computational Crystallography Toolbox( cctbx) to overcome these challenges. Accurate unit-cell information derived from an aggregate data set from thousands of diffraction patterns can be used to determine a crystal orientation matrix for individual images with as few as five reflections. These algorithms are potentially applicable not only to amyloid peptides but also to any set ofmore » diffraction patterns with sparse properties, such as low-resolution virus structures or high-throughput screening of still images captured by raster-scanning at synchrotron sources. As a proof of concept for this technique, successful integration of X-ray free-electron laser (XFEL) data to 2.5 Å resolution for the amyloid segment GNNQQNY from the Sup35 yeast prion is presented.« less

Scattering apodizer for laser beams

DOEpatents

Summers, Mark A.; Hagen, Wilhelm F.; Boyd, Robert D.

1985-01-01

A method is disclosed for apodizing a laser beam to smooth out the production of diffraction peaks due to optical discontinuities in the path of the laser beam, such method comprising introduction of a pattern of scattering elements for reducing the peak intensity in the region of such optical discontinuities, such pattern having smoothly tapering boundaries in which the distribution density of the scattering elements is tapered gradually to produce small gradients in the distribution density, such pattern of scattering elements being effective to reduce and smooth out the diffraction effects which would otherwise be produced. The apodizer pattern may be produced by selectively blasting a surface of a transparent member with fine abrasive particles to produce a multitude of minute pits. In one embodiment, a scattering apodizer pattern is employed to overcome diffraction patterns in a multiple element crystal array for harmonic conversion of a laser beam. The interstices and the supporting grid between the crystal elements are obscured by the gradually tapered apodizer pattern of scattering elements.

Scattering apodizer for laser beams

DOEpatents

Summers, M.A.; Hagen, W.F.; Boyd, R.D.

1984-01-01

A method is disclosed for apodizing a laser beam to smooth out the production of diffraction peaks due to optical discontinuities in the path of the laser beam, such method comprising introduction of a pattern of scattering elements for reducing the peak intensity in the region of such optical discontinuities, such pattern having smoothly tapering boundaries in which the distribution density of the scattering elements is tapered gradually to produce small gradients in the distribution density, such pattern of scattering elements being effective to reduce and smooth out the diffraction effects which would otherwise be produced. The apodizer pattern may be produced by selectively blasting a surface of a transparent member with fine abrasive particles to produce a multitude of minute pits. In one embodiment, a scattering apodizer pattern is employed to overcome diffraction patterns in a multiple element crystal array for harmonic conversion of a laser beam. The interstices and the supporting grid between the crystal elements are obscured by the gradually tapered apodizer pattern of scattering elements.

Undergraduate Experiment with Fractal Diffraction Gratings

ERIC Educational Resources Information Center

Monsoriu, Juan A.; Furlan, Walter D.; Pons, Amparo; Barreiro, Juan C.; Gimenez, Marcos H.

2011-01-01

We present a simple diffraction experiment with fractal gratings based on the triadic Cantor set. Diffraction by fractals is proposed as a motivating strategy for students of optics in the potential applications of optical processing. Fraunhofer diffraction patterns are obtained using standard equipment present in most undergraduate physics…

Synthesis, structural characterization, DFT studies and in-vitro antidiabetic activity of new mixed ligand oxovanadium(IV) complex with tridentate Schiff base

NASA Astrophysics Data System (ADS)

Patel, R. N.; Singh, Yogendra Pratap

2018-02-01

The mixed ligand oxovanadium(IV) complex [VO(L1)(L2)] [L1 = N'-[(Z)-phenyl(pyridin-2-yl)methylidene]benzohydrazide and L2 = Benzohydrazide] has been synthesized in aerobic condition. The complex was characterized by elemental analysis spectroscopic (UV-vis, IR, epr) and electrochemical methods. X-ray diffraction pattern was also used to characterize this complex, which has a distorted octahedral structure. Single crystal diffraction analysis reveals that Csbnd H⋯π (aryl/metal chelate rings) interactions contribute to the stabilization of the crystal structure in given dimension. The room temperature magnetic susceptibility data shows paramagnetic nature of the complex. The complex was also tested for in-vitro antidiabetic activity. Moderate α-glucosidase inhibition is shown by this complex, which may be considered as α-glucosidase inhibitors.

Synthesis of Large-grain, Single-crystalline Monolayer and AB-stacking Bilayer Graphene

NASA Astrophysics Data System (ADS)

Zhang, Luyao; Lin, Yung-Chen; Zhang, Yi; Chang, Han-Wen; Yeh, Wen-Cheng; Zhou, Chongwu; USC Nanotechnology Research Laboratory Team

2013-03-01

We report the growth of large-grain, single-crystalline monolayer and AB-stacking bilayer graphene by the combination of ambient pressure chemical vapor deposition and low pressure chemical vapor deposition. The shape of the monolayer graphene was modified to be either hexagons or flowers under different growth conditions. The size of the bilayer graphene region was enlarged under ambient pressure growth conditions with low methane concentration. Raman spectra and selected area electron diffraction of individual graphene grain indicated that the each graphene grain is single-crystalline. With electron beam lithography patterned PMMA seeds, graphene nucleation can be controlled and graphene monolayer and bilayer arrays were synthesized on copper foil. Electron backscatter diffraction study revealed that the graphene morphology had little correlation with the crystalline orientation of underlying copper substrate. Mork Family Department of Chemical Engineering and Materials Science

Impedance spectroscopic and dielectric properties of nanosized Y2/3Cu3Ti4O12 ceramic

NASA Astrophysics Data System (ADS)

Sharma, Sunita; Yadav, Shiv Sundar; Singh, M. M.; Mandal, K. D.

2014-11-01

Yttrium Copper Titanate (Y2/3Cu3Ti4O12) nanoceramic is structurally analogous to CaCu3Ti4O12 (CCTO). X-ray diffraction (XRD) of Y2/3Cu3Ti4O12 (YCTO) shows the presence of all normal peaks of CCTO. SEM micrograph exhibits the presence of bimodal grains of size ranging from 1-2 μm. Bright field TEM image clearly displays nanocrystalline particle which is supported by presence of a few clear rings in the corresponding selected area electron diffraction (SAED) pattern. It exhibits a high value of dielectric constant (ɛ‧ = 8434) at room temperature and 100 Hz frequency with characteristic relaxation peaks. Impedance and modulus studies revealed the presence of temperature-dependent Maxwell-Wagner type of relaxation in the ceramic.

Structural, electrical, optical and magnetic properties of NiO/ZnO thin films

NASA Astrophysics Data System (ADS)

Sushmitha, V.; Maragatham, V.; Raj, P. Deepak; Sridharan, M.

2018-02-01

Nickel oxide/Zinc oxide (NiO/ZnO) thin films have been deposited onto thoroughly cleaned glass substrates by reactive direct current (DC) magnetron sputtering technique and subsequently annealed at 300 °C for 3 h in vacuum. The NiO/ZnO thin films were then studied for their structural, optical and electrical properties. X-ray diffraction (XRD) pattern of ZnO and NiO showed the diffraction planes corresponding to hexagonal and cubic phase respectively. The optical properties showed that with the increase in the deposition time of NiO the energy band gap varied between 3.1 to 3.24 eV. Hence, by changing the deposition time of NiO the tuning of band gap and conductivity were achieved. The magnetic studies revealed the diamagnetic nature of the NiO/ZnO thin films.

Erratum to: Psammoma bodies in two types of human ovarian tumours: a mineralogical study

NASA Astrophysics Data System (ADS)

Meng, Fanlu; Wang, Changqiu; Li, Yan; Lu, Anhuai; Mei, Fang; Liu, Jianying; Du, Jingyun; Zhang, Yan

2015-06-01

Psammoma body (PB) is a common form of calcification in pathological diagnosis and closely relevant to tumours. This paper focuses on the mineralogical characteristics of PBs in ovarian serous cancer and teratoma by using polarization microscope (POM), environmental scanning electron microscope (ESEM), micro-Fourier transform infrared spectroscopy (micro-FT-IR), transmission electron microscope (TEM), micro-area synchrotron radiation X-ray powder diffraction (μ-SRXRD) and fluorescence (μ-SRXRF). Both the PBs in tissues and separated from eight typical cases were investigated. POM and ESEM observation revealed the inside-out growth pattern of PBs. μ-SRXRD and micro-FT-IR results demonstrated the dominant mineral phase of PBs in ovarian serous cancer and teratoma was AB-type carbonate hydroxyapatite (Ca10[(PO4)6-x-y(CO3)x(HPO4)y][(OH)2-u(CO3)u] with 0 ≤ x,y,u ≤ 2). As observed by ESEM and TEM, the layer-rich PBs in teratoma were up to 70 μm and mainly consisted of 5 nm-wide, 5-12 nm-long columnar crystals; the PBs in ovarian serous cancer with a maximum diameter of 35 μm were composed of slightly longer columnar crystals and granulates with 20-100 nm in diameter. The selected area electron diffraction patterns showed dispersed polycrystalline diffraction rings with arching behavior of (002) diffraction, indicating the aggregated nanocrystals grew in the preferred orientation of (002) face. The EDX and μ-SRXRF results together indicated the existence of Na, Mg, Zn and Sr in PBs. These detailed mineralogical characteristics may help uncover the nature of the pathological PBs in ovary.

Psammoma bodies in two types of human ovarian tumours: a mineralogical study

NASA Astrophysics Data System (ADS)

Fanlu, Meng; Changqiu, Wang; Yan, Li; Anhuai, Lu; Fang, Mei; Jianying, Liu; Jingyun, Du; Yan, Zhang

2015-06-01

Psammoma body (PB) is a common form of calcification in pathological diagnosis and closely relevant to tumours. This paper focuses on the mineralogical characteristics of PBs in ovarian serous cancer and teratoma by using polarization microscope (POM), environmental scanning electron microscope (ESEM), micro-Fourier transform infrared spectroscopy (micro-FT-IR), transmission electron microscope (TEM), micro-area synchrotron radiation X-ray powder diffraction (μ-SRXRD) and fluorescence (μ-SRXRF). Both the PBs in tissues and separated from eight typical cases were investigated. POM and ESEM observation revealed the inside-out growth pattern of PBs. μ-SRXRD and micro-FT-IR results demonstrated the dominant mineral phase of PBs in ovarian serous cancer and teratoma was AB-type carbonate hydroxyapatite (Ca10[(PO4)6-x-y(CO3)x(HPO4 2-)y][(OH)2-u(CO3)u] with 0 ≤ x,y,u ≤ 2). As observed by ESEM and TEM, the layer-rich PBs in teratoma were up to 70 μm and mainly consisted of 5 nm-wide, 5-12 nm-long columnar crystals; the PBs in ovarian serous cancer with a maximum diameter of 35 μm were composed of slightly longer columnar crystals and granulates with 20-100 nm in diameter. The selected area electron diffraction patterns showed dispersed polycrystalline diffraction rings with arching behavior of (002) diffraction, indicating the aggregated nanocrystals grew in the preferred orientation of (002) face. The EDX and μ-SRXRF results together indicated the existence of Na, Mg, Zn and Sr in PBs. These detailed mineralogical characteristics may help uncover the nature of the pathological PBs in ovary.

Uric Acid Spherulites in the Reflector Layer of Firefly Light Organ

PubMed Central

Goh, King-Siang; Sheu, Hwo-Shuenn; Hua, Tzu-En; Kang, Mei-Hua; Li, Chia-Wei

2013-01-01

Background In firefly light organs, reflector layer is a specialized tissue which is believed to play a key role for increasing the bioluminescence intensity through reflection. However, the nature of this unique tissue remains elusive. In this report, we investigated the role, fine structure and nature of the reflector layer in the light organ of adult Luciola cerata. Principal Findings Our results indicated that the reflector layer is capable of reflecting bioluminescence, and contains abundant uric acid. Electron microscopy (EM) demonstrated that the cytosol of the reflector layer's cells is filled with densely packed spherical granules, which should be the uric acid granules. These granules are highly regular in size (∼700 nm in diameter), and exhibit a radial internal structure. X-ray diffraction (XRD) analyses revealed that an intense single peak pattern with a d-spacing value of 0.320 nm is specifically detected in the light organ, and is highly similar to the diffraction peak pattern and d-spacing value of needle-formed crystals of monosodium urate monohydrate. However, the molar ratio evaluation of uric acid to various cations (K+, Na+, Ca2+ and Mg2+) in the light organ deduced that only a few uric acid molecules were in the form of urate salts. Thus, non-salt uric acid should be the source of the diffraction signal detected in the light organ. Conclusions In the light organ, the intense single peak diffraction signal might come from a unique needle-like uric acid form, which is different from other known structures of non-salt uric acid form. The finding of a radial structure in the granules of reflector layer implies that the spherical uric acid granules might be formed by the radial arrangement of needle-formed packing matter. PMID:23441187

Structure analysis of the single-domain Si(111)4 × 1-In surface by μ-probe Auger electron diffraction and μ-probe reflection high energy electron diffraction

NASA Astrophysics Data System (ADS)

Nakamura, N.; Anno, K.; Kono, S.

1991-10-01

A single-domain Si(111)4 × 1-In surface has been studied by μ-probe reflection high-energy electron diffraction (RHEED) to elucidate the symmetry of the 4 × 1 surface. Azimuthal diffraction patterns of In MNN Auger electron have been obtained by a μ-probe Auger electron diffraction (AED) apparatus from the single-domain Si(111)4 × 1-In surface. On the basis of information from scanning tunneling microscopy [J. Microsc. 152 (1988) 727] and under the assumption that the 4 × 1 surface is composed of In-overlayers, the μ-probe AED patterns were kinematically analyzed to reach a concrete model of indium arrangement.

X-Ray Diffraction Apparatus

NASA Technical Reports Server (NTRS)

Blake, David F. (Inventor); Bryson, Charles (Inventor); Freund, Friedmann (Inventor)

1996-01-01

An x-ray diffraction apparatus for use in analyzing the x-ray diffraction pattern of a sample is introduced. The apparatus includes a beam source for generating a collimated x-ray beam having one or more discrete x-ray energies, a holder for holding the sample to be analyzed in the path of the beam, and a charge-coupled device having an array of pixels for detecting, in one or more selected photon energy ranges, x-ray diffraction photons produced by irradiating such a sample with said beam. The CCD is coupled to an output unit which receives input information relating to the energies of photons striking each pixel in the CCD, and constructs the diffraction pattern of photons within a selected energy range striking the CCD.

High-resolution three-dimensional partially coherent diffraction imaging.

PubMed

Clark, J N; Huang, X; Harder, R; Robinson, I K

2012-01-01

The wave properties of light, particularly its coherence, are responsible for interference effects, which can be exploited in powerful imaging applications. Coherent diffractive imaging relies heavily on coherence and has recently experienced rapid growth. Coherent diffractive imaging recovers an object from its diffraction pattern by computational phasing with the potential of wavelength-limited resolution. Diminished coherence results in reconstructions that suffer from artefacts or fail completely. Here we demonstrate ab initio phasing of partially coherent diffraction patterns in three dimensions, while simultaneously determining the coherence properties of the illuminating wavefield. Both the dramatic improvements in image interpretability and the three-dimensional evaluation of the coherence will have broad implications for quantitative imaging of nanostructures and wavefield characterization with X-rays and electrons.

Common arc method for diffraction pattern orientation.

PubMed

Bortel, Gábor; Tegze, Miklós

2011-11-01

Very short pulses of X-ray free-electron lasers opened the way to obtaining diffraction signal from single particles beyond the radiation dose limit. For three-dimensional structure reconstruction many patterns are recorded in the object's unknown orientation. A method is described for the orientation of continuous diffraction patterns of non-periodic objects, utilizing intensity correlations in the curved intersections of the corresponding Ewald spheres, and hence named the common arc orientation method. The present implementation of the algorithm optionally takes into account Friedel's law, handles missing data and is capable of determining the point group of symmetric objects. Its performance is demonstrated on simulated diffraction data sets and verification of the results indicates a high orientation accuracy even at low signal levels. The common arc method fills a gap in the wide palette of orientation methods. © 2011 International Union of Crystallography

Three-dimensional reconstruction for coherent diffraction patterns obtained by XFEL.

PubMed

Nakano, Miki; Miyashita, Osamu; Jonic, Slavica; Song, Changyong; Nam, Daewoong; Joti, Yasumasa; Tama, Florence

2017-07-01

The three-dimensional (3D) structural analysis of single particles using an X-ray free-electron laser (XFEL) is a new structural biology technique that enables observations of molecules that are difficult to crystallize, such as flexible biomolecular complexes and living tissue in the state close to physiological conditions. In order to restore the 3D structure from the diffraction patterns obtained by the XFEL, computational algorithms are necessary as the orientation of the incident beam with respect to the sample needs to be estimated. A program package for XFEL single-particle analysis based on the Xmipp software package, that is commonly used for image processing in 3D cryo-electron microscopy, has been developed. The reconstruction program has been tested using diffraction patterns of an aerosol nanoparticle obtained by tomographic coherent X-ray diffraction microscopy.

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl(6) and other alloys are twinned cubic crystals.

PubMed

Pauling, L

1987-06-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl(6) and Mg(32)(Al,Zn)(49) and the neutron powder diffraction pattern of MnAl(6) are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 A (x-ray) and 23.416 A (neutron) for MnAl(6) and 24.313 A (x-ray) for Mg(32)(Al,Zn)(49).

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl6 and other alloys are twinned cubic crystals

PubMed Central

Pauling, Linus

1987-01-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl6 and Mg32(Al,Zn)49 and the neutron powder diffraction pattern of MnAl6 are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 Å (x-ray) and 23.416 Å (neutron) for MnAl6 and 24.313 Å (x-ray) for Mg32(Al,Zn)49. PMID:16593841

Electrochemically synthesis and optoelectronic properties of Pb- and Zn-doped nanostructured SnSe films

NASA Astrophysics Data System (ADS)

Jamali-Sheini, Farid; Cheraghizade, Mohsen; Yousefi, Ramin

2018-06-01

In this study, electrodeposition technique was applied to deposit un-, lead (Pb), and zinc (Zn)-doped SnSe films. X-ray diffraction (XRD) patterns of the films showed a polycrystalline SnSe phase with orthorhombic crystalline lattice. SEM images revealed ball-shaped, rod-shaped, and wire-shaped morphologies for SnSe films. Moreover, optical measurements indicated incorporation of dopant in the crystalline lattice of films by varying the optical energy band gap. Electrical characterization of Pb- and Zn-doped SnSe films showed their p-type nature. Finally, the solar cell device fabricated using the Zn-doped SnSe films reveal a higher efficiency because of their higher carrier concentration.

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.

Quantum dynamical simulation of the scattering of Ar from a frozen LiF(100) surface based on a first principles interaction potential

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

Azuri, Asaf; Pollak, Eli, E-mail: eli.pollak@weizmann.ac.il

2015-07-07

In-plane two and three dimensional diffraction patterns are computed for the vertical scattering of an Ar atom from a frozen LiF(100) surface. Suitable collimation of the incoming wavepacket serves to reveal the quantum mechanical diffraction. The interaction potential is based on a fit to an ab initio potential calculated using density functional theory with dispersion corrections. Due to the potential coupling found between the two horizontal surface directions, there are noticeable differences between the quantum angular distributions computed for two and three dimensional scattering. The quantum results are compared to analogous classical Wigner computations on the same surface and withmore » the same conditions. The classical dynamics largely provides the envelope for the quantum diffractive scattering. The classical results also show that the corrugation along the [110] direction of the surface is smaller than along the [100] direction, in qualitative agreement with experimental observations of unimodal and bimodal scattering for the [110] and [100] directions, respectively.« less

Synthesis and characterization of graphene oxide using modified Hummer's method

NASA Astrophysics Data System (ADS)

Kaur, Manpreet; Kaur, Harsimran; Kukkar, Deepak

2018-05-01

In the present study, a simple approach has been followed for the synthesis of graphene oxide (GO) using modified Hummers method in which graphite powder was oxidized in the presence of concentrated H2SO4 and KMnO4. The amount of NaNO3 and KMnO4 was varied to produce sheet like structure. The varied concentrations of NaNO3 and KMnO4 resulted in yielding large amount of the product. Structural, morphological and physicochemical features of the product were studied using UV-Visible spectrophotometer, Fourier Transform infrared spectroscopy (FTIR), and crystal structure was determined using X-ray powder diffraction (XRD). UV-Vis spectra of GO was observed at a maximum absorption of 230 nm due to (π-π*) transition of atomic carbon-carbon bonds. FTIR spectra revealed the presence of oxygen containing functional groups which ensures the complete exfoliation of graphite into graphene oxide X-ray powder diffraction pattern of the product showed the diffraction peak at (2θ = 26.7°) with an interlayer spacing of 0.334 nm. All the above characterizations successfully confirmed the formation of GO.

Three-dimensional coherent X-ray diffractive imaging of whole frozen-hydrated cells

PubMed Central

Rodriguez, Jose A.; Xu, Rui; Chen, Chien-Chun; Huang, Zhifeng; Jiang, Huaidong; Chen, Allan L.; Raines, Kevin S.; Pryor Jr, Alan; Nam, Daewoong; Wiegart, Lutz; Song, Changyong; Madsen, Anders; Chushkin, Yuriy; Zontone, Federico; Bradley, Peter J.; Miao, Jianwei

2015-01-01

A structural understanding of whole cells in three dimensions at high spatial resolution remains a significant challenge and, in the case of X-rays, has been limited by radiation damage. By alleviating this limitation, cryogenic coherent diffractive imaging (cryo-CDI) can in principle be used to bridge the important resolution gap between optical and electron microscopy in bio-imaging. Here, the first experimental demonstration of cryo-CDI for quantitative three-dimensional imaging of whole frozen-hydrated cells using 8 keV X-rays is reported. As a proof of principle, a tilt series of 72 diffraction patterns was collected from a frozen-hydrated Neospora caninum cell and the three-dimensional mass density of the cell was reconstructed and quantified based on its natural contrast. This three-dimensional reconstruction reveals the surface and internal morphology of the cell, including its complex polarized sub-cellular structure. It is believed that this work represents an experimental milestone towards routine quantitative three-dimensional imaging of whole cells in their natural state with spatial resolutions in the tens of nanometres. PMID:26306199

Three-dimensional coherent X-ray diffractive imaging of whole frozen-hydrated cells

DOE PAGES

Rodriguez, Jose A.; Xu, Rui; Chen, Chien -Chun; ...

2015-09-01

Here, a structural understanding of whole cells in three dimensions at high spatial resolution remains a significant challenge and, in the case of X-rays, has been limited by radiation damage. By alleviating this limitation, cryogenic coherent diffractive imaging (cryo-CDI) can in principle be used to bridge the important resolution gap between optical and electron microscopy in bio-imaging. Here, the first experimental demonstration of cryo-CDI for quantitative three-dimensional imaging of whole frozen-hydrated cells using 8 Kev X-rays is reported. As a proof of principle, a tilt series of 72 diffraction patterns was collected from a frozen-hydrated Neospora caninum cell and themore » three-dimensional mass density of the cell was reconstructed and quantified based on its natural contrast. This three-dimensional reconstruction reveals the surface and internal morphology of the cell, including its complex polarized sub-cellular structure. Finally, it is believed that this work represents an experimental milestone towards routine quantitative three-dimensional imaging of whole cells in their natural state with spatial resolutions in the tens of nanometres.« less

Crystallization and preliminary X-ray analysis of a low density lipoprotein from human plasma.

PubMed

Prassl, R; Chapman, J M; Nigon, F; Sara, M; Eschenburg, S; Betzel, C; Saxena, A; Laggner, P

1996-11-15

Single crystals of human plasma low density lipoprotein (LDL), the major transport vehicle for cholesterol in blood, have been produced with a view to analysis of the three-dimensional structure by x-ray crystallography. Crystals with dimensions of approximately 200 x 100 x 50 microm have been reproducibly obtained from highly homogeneous LDL particle subspecies, isolated in the density ranges d = 1.0271-1. 0297 g/ml and d = 1.0297-1.0327 g/ml. Electron microscopic imaging of ultrathin-sectioned preparations of the crystals confirmed the existence of a regular, quasihexagonal arrangement of spherical particles of approximately 18 nm in diameter, thereby resembling the dimensions characteristic of LDL after dehydration and fixation. X-ray diffraction with synchrotron radiation under cryogenic conditions revealed the presence of well resolved diffraction spots, to a resolution of about 29 A. The diffraction patterns are indexed in terms of a triclinic lattice with unit cell dimensions of a = 16. 1 nm, b = 39.0 nm, c = 43.9 nm; alpha = 96.2 degrees, beta = 92.1 degrees, gamma = 102 degrees, and with space group P1.

Three-dimensional coherent X-ray diffractive imaging of whole frozen-hydrated cells.

PubMed

Rodriguez, Jose A; Xu, Rui; Chen, Chien-Chun; Huang, Zhifeng; Jiang, Huaidong; Chen, Allan L; Raines, Kevin S; Pryor, Alan; Nam, Daewoong; Wiegart, Lutz; Song, Changyong; Madsen, Anders; Chushkin, Yuriy; Zontone, Federico; Bradley, Peter J; Miao, Jianwei

2015-09-01

A structural understanding of whole cells in three dimensions at high spatial resolution remains a significant challenge and, in the case of X-rays, has been limited by radiation damage. By alleviating this limitation, cryogenic coherent diffractive imaging (cryo-CDI) can in principle be used to bridge the important resolution gap between optical and electron microscopy in bio-imaging. Here, the first experimental demonstration of cryo-CDI for quantitative three-dimensional imaging of whole frozen-hydrated cells using 8 keV X-rays is reported. As a proof of principle, a tilt series of 72 diffraction patterns was collected from a frozen-hydrated Neospora caninum cell and the three-dimensional mass density of the cell was reconstructed and quantified based on its natural contrast. This three-dimensional reconstruction reveals the surface and internal morphology of the cell, including its complex polarized sub-cellular structure. It is believed that this work represents an experimental milestone towards routine quantitative three-dimensional imaging of whole cells in their natural state with spatial resolutions in the tens of nanometres.

Structure of naturally hydrated ferrihydrite revealed through neutron diffraction and first-principles modeling

NASA Astrophysics Data System (ADS)

Chappell, Helen F.; Thom, William; Bowron, Daniel T.; Faria, Nuno; Hasnip, Philip J.; Powell, Jonathan J.

2017-08-01

Ferrihydrite, with a ``two-line'' x-ray diffraction pattern (2L-Fh), is the most amorphous of the iron oxides and is ubiquitous in both terrestrial and aquatic environments. It also plays a central role in the regulation and metabolism of iron in bacteria, algae, higher plants, and animals, including humans. In this study, we present a single-phase model for ferrihydrite that unifies existing analytical data while adhering to fundamental chemical principles. The primary particle is small (20-50 Å) and has a dynamic and variably hydrated surface, which negates long-range order; collectively, these features have hampered complete characterization and frustrated our understanding of the mineral's reactivity and chemical/biochemical function. Near and intermediate range neutron diffraction (NIMROD) and first-principles density functional theory (DFT) were employed in this study to generate and interpret high-resolution data of naturally hydrated, synthetic 2L-Fh at standard temperature. The structural optimization overcomes transgressions of coordination chemistry inherent within previously proposed structures, to produce a robust and unambiguous single-phase model.

Dual-color STED microscopy reveals a sandwich structure of Bassoon and Piccolo in active zones of adult and aged mice.

PubMed

Nishimune, Hiroshi; Badawi, Yomna; Mori, Shuuichi; Shigemoto, Kazuhiro

2016-06-20

Presynaptic active zones play a pivotal role as synaptic vesicle release sites for synaptic transmission, but the molecular architecture of active zones in mammalian neuromuscular junctions (NMJs) at sub-diffraction limited resolution remains unknown. Bassoon and Piccolo are active zone specific cytosolic proteins essential for active zone assembly in NMJs, ribbon synapses, and brain synapses. These proteins are thought to colocalize and share some functions at active zones. Here, we report an unexpected finding of non-overlapping localization of these two proteins in mouse NMJs revealed using dual-color stimulated emission depletion (STED) super resolution microscopy. Piccolo puncta sandwiched Bassoon puncta and aligned in a Piccolo-Bassoon-Piccolo structure in adult NMJs. P/Q-type voltage-gated calcium channel (VGCC) puncta colocalized with Bassoon puncta. The P/Q-type VGCC and Bassoon protein levels decreased significantly in NMJs from aged mouse. In contrast, the Piccolo levels in NMJs from aged mice were comparable to levels in adult mice. This study revealed the molecular architecture of active zones in mouse NMJs at sub-diffraction limited resolution, and described the selective degeneration mechanism of active zone proteins in NMJs from aged mice. Interestingly, the localization pattern of active zone proteins described herein is similar to active zone structures described using electron microscope tomography.

An amyloid-forming peptide from the yeast prion Sup35 reveals a dehydrated β-sheet structure for amyloid

PubMed Central

Balbirnie, Melinda; Grothe, Robert; Eisenberg, David S.

2001-01-01

X-ray diffraction and other biophysical tools reveal features of the atomic structure of an amyloid-like crystal. Sup35, a prion-like protein in yeast, forms fibrillar amyloid assemblies intrinsic to its prion function. We have identified a polar peptide from the N-terminal prion-determining domain of Sup35 that exhibits the amyloid properties of full-length Sup35, including cooperative kinetics of aggregation, fibril formation, binding of the dye Congo red, and the characteristic cross-β x-ray diffraction pattern. Microcrystals of this peptide also share the principal properties of the fibrillar amyloid, including a highly stable, β-sheet-rich structure and the binding of Congo red. The x-ray powder pattern of the microcrystals, extending to 0.9-Å resolution, yields the unit cell dimensions of the well-ordered structure. These dimensions restrict possible atomic models of this amyloid-like structure and demonstrate that it forms packed, parallel-stranded β-sheets. The unusually high density of the crystals shows that the packed β-sheets are dehydrated, despite the polar character of the side chains. These results suggest that amyloid is a highly intermolecularly bonded, dehydrated array of densely packed β-sheets. This dry β-sheet could form as Sup35 partially unfolds to expose the peptide, permitting it to hydrogen-bond to the same peptide of other Sup35 molecules. The implication is that amyloid-forming units may be short segments of proteins, exposed for interactions by partial unfolding. PMID:11226247

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.

3D Diffraction Microscope Provides a First Deep View

NASA Astrophysics Data System (ADS)

Miao, Jianwei

2005-03-01

When a coherent diffraction pattern is sampled at a spacing sufficiently finer than the Bragg peak frequency (i.e. the inverse of the sample size), the phase information is in principle encoded inside the diffraction pattern, and can be directly retrieved by using an iterative process. In combination of this oversampling phasing method with either coherent X-rays or electrons, a novel form of diffraction microscopy has recently been developed to image nanoscale materials and biological structures. In this talk, I will present the principle of the oversampling method, discuss the first experimental demonstration of this microscope, and illustrate some applications in nanoscience and biology.

Hair treatment process providing dispersed colors by light diffraction

DOEpatents

Sutton, Richard Matthew Charles; Lamartine, Bruce Carvell; Orler, E. Bruce; Song, Shuangqi

2015-12-22

A hair treatment process for providing dispersed colors by light diffraction including (a) coating the hair with a material comprising a polymer, (b) pressing the hair with a pressing device including one or more surfaces, and (c) forming a secondary nanostructured surface pattern on the hair that is complementary to the primary nanostructured surface pattern on the one or more surfaces of the pressing device. The secondary nanostructured surface pattern diffracts light into dispersed colors that are visible on the hair. The section of the hair is pressed with the pressing device for from about 1 to 55 seconds. The polymer has a glass transition temperature from about 55.degree. C. to about 90.degree. C. The one or more surfaces include a primary nanostructured surface pattern.

A Combined FEM/MoM/GTD Technique To Analyze Elliptically Polarized Cavity-Backed Antennas With Finite Ground Plane

NASA Technical Reports Server (NTRS)

Reddy, C. J.; Deshpande, M. D.; Fralick, D. T.; Cockrell, C. R.; Beck, F. B.

1996-01-01

Radiation pattern prediction analysis of elliptically polarized cavity-backed aperture antennas in a finite ground plane is performed using a combined Finite Element Method/Method of Moments/Geometrical Theory of Diffraction (FEM/MoM/GTD) technique. The magnetic current on the cavity-backed aperture in an infinite ground plane is calculated using the combined FEM/MoM analysis. GTD, including the slope diffraction contribution, is used to calculate the diffracted fields caused by both soft and hard polarizations at the edges of the finite ground plane. Explicit expressions for regular diffraction coefficients and slope diffraction coefficients are presented. The slope of the incident magnetic field at the diffraction points is derived and analytical expressions are presented. Numerical results for the radiation patterns of a cavity-backed circular spiral microstrip patch antenna excited by a coaxial probe in a finite rectangular ground plane are computed and compared with experimental results.

Multiple defocused coherent diffraction imaging: method for simultaneously reconstructing objects and probe using X-ray free-electron lasers.

PubMed

Hirose, Makoto; Shimomura, Kei; Suzuki, Akihiro; Burdet, Nicolas; Takahashi, Yukio

2016-05-30

The sample size must be less than the diffraction-limited focal spot size of the incident beam in single-shot coherent X-ray diffraction imaging (CXDI) based on a diffract-before-destruction scheme using X-ray free electron lasers (XFELs). This is currently a major limitation preventing its wider applications. We here propose multiple defocused CXDI, in which isolated objects are sequentially illuminated with a divergent beam larger than the objects and the coherent diffraction pattern of each object is recorded. This method can simultaneously reconstruct both objects and a probe from the coherent X-ray diffraction patterns without any a priori knowledge. We performed a computer simulation of the prposed method and then successfully demonstrated it in a proof-of-principle experiment at SPring-8. The prposed method allows us to not only observe broad samples but also characterize focused XFEL beams.

HiSPoD: a program for high-speed polychromatic X-ray diffraction experiments and data analysis on polycrystalline samples

DOE PAGES

Sun, Tao; Fezzaa, Kamel

2016-06-17

Here, a high-speed X-ray diffraction technique was recently developed at the 32-ID-B beamline of the Advanced Photon Source for studying highly dynamic, yet non-repeatable and irreversible, materials processes. In experiments, the microstructure evolution in a single material event is probed by recording a series of diffraction patterns with extremely short exposure time and high frame rate. Owing to the limited flux in a short pulse and the polychromatic nature of the incident X-rays, analysis of the diffraction data is challenging. Here, HiSPoD, a stand-alone Matlab-based software for analyzing the polychromatic X-ray diffraction data from polycrystalline samples, is described. With HiSPoD,more » researchers are able to perform diffraction peak indexing, extraction of one-dimensional intensity profiles by integrating a two-dimensional diffraction pattern, and, more importantly, quantitative numerical simulations to obtain precise sample structure information.« less

Reentrant cluster glass and stability of ferromagnetism in the Ga2MnCo Heusler alloy

NASA Astrophysics Data System (ADS)

Samanta, Tamalika; Bhobe, P. A.; Das, A.; Kumar, A.; Nigam, A. K.

2018-05-01

We present here a detailed investigation into the magnetic ordering of a full Heusler alloy Ga2MnCo using dc and ac magnetization measurements, neutron diffraction, and neutron depolarization experiments. The crystal structure at room temperature was first confirmed to be L 21 using the highly intense synchrotron x-ray diffraction technique. Temperature-dependent magnetization reveals that Ga2MnCo enters a ferromagnetic (FM) state at TC=154 K, characterized by a sharp increase in magnetization and a plateaulike region hereafter. As the temperature is decreased further, a sharp drop in magnetization is observed at Tf=50 K, hinting toward an antiferromagnetic (AFM) phase change. Neutron diffraction (ND) recorded over the range of temperature from 6 to 300 K provides combined information regarding crystal as well as magnetic structure. Accordingly, an increase in the intensity of the ND pattern is seen at 150 K, signaling the onset of long-range FM order. However, there is no sign of the appearance of superlattice reflections corresponding to the AFM phase in the patterns recorded below 50 K. An unusual discontinuity in the unit-cell volume is seen around Tf, indicating a coupling of this second transition with the contraction of the lattice. Attempts to unravel this interesting magnetic behavior using ac susceptibility measurements led to the existence of glassy magnetism below Tf. Systematic analysis of the susceptibility results along with neutron depolarization measurement identifies the low-temperature phase as a reentrant cluster glass.

rf streak camera based ultrafast relativistic electron diffraction.

PubMed

Musumeci, P; Moody, J T; Scoby, C M; Gutierrez, M S; Tran, T

2009-01-01

We theoretically and experimentally investigate the possibility of using a rf streak camera to time resolve in a single shot structural changes at the sub-100 fs time scale via relativistic electron diffraction. We experimentally tested this novel concept at the UCLA Pegasus rf photoinjector. Time-resolved diffraction patterns from thin Al foil are recorded. Averaging over 50 shots is required in order to get statistics sufficient to uncover a variation in time of the diffraction patterns. In the absence of an external pump laser, this is explained as due to the energy chirp on the beam out of the electron gun. With further improvements to the electron source, rf streak camera based ultrafast electron diffraction has the potential to yield truly single shot measurements of ultrafast processes.

Coherent Bragg nanodiffraction at the hard X-ray Nanoprobe beamline.

PubMed

Hruszkewycz, S O; Holt, M V; Maser, J; Murray, C E; Highland, M J; Folkman, C M; Fuoss, P H

2014-03-06

Bragg coherent diffraction with nanofocused hard X-ray beams provides unique opportunities for quantitative in situ studies of crystalline structure in nanoscale regions of complex materials and devices by a variety of diffraction-based techniques. In the case of coherent diffraction imaging, a major experimental challenge in using nanoscale coherent beams is maintaining a constant scattering volume such that coherent fringe visibility is maximized and maintained over the course of an exposure lasting several seconds. Here, we present coherent Bragg diffraction patterns measured from different nanostructured thin films at the Sector 26 Nanoprobe beamline at the Advanced Photon Source and demonstrate that with nanoscale positional control, coherent diffraction patterns can be measured with source-limited fringe visibilities more than 50% suitable for imaging by coherent Bragg ptychography techniques.

Coherent Bragg nanodiffraction at the hard X-ray Nanoprobe beamline

PubMed Central

Hruszkewycz, S. O.; Holt, M. V.; Maser, J.; Murray, C. E.; Highland, M. J.; Folkman, C. M.; Fuoss, P. H.

2014-01-01

Bragg coherent diffraction with nanofocused hard X-ray beams provides unique opportunities for quantitative in situ studies of crystalline structure in nanoscale regions of complex materials and devices by a variety of diffraction-based techniques. In the case of coherent diffraction imaging, a major experimental challenge in using nanoscale coherent beams is maintaining a constant scattering volume such that coherent fringe visibility is maximized and maintained over the course of an exposure lasting several seconds. Here, we present coherent Bragg diffraction patterns measured from different nanostructured thin films at the Sector 26 Nanoprobe beamline at the Advanced Photon Source and demonstrate that with nanoscale positional control, coherent diffraction patterns can be measured with source-limited fringe visibilities more than 50% suitable for imaging by coherent Bragg ptychography techniques. PMID:24470418

Diffraction of entangled particles by light gratings

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

Sancho, Pedro, E-mail: psanchos@aemet.es

We analyze the diffraction regime of the Kapitza–Dirac effect for particles entangled in momentum. The detection patterns show two-particle interferences. In the single-mode case we identify a discontinuity in the set of joint detection probabilities, associated with the disconnected character of the space of non-separable states. For Gaussian multi-mode states we derive the diffraction patterns, providing an example of the dependence of the light–matter interaction on entanglement. When the particles are identical, we can explore the relation between exchange and entanglement effects. We find a complementary behavior between overlapping and Schmidt’s number. In particular, symmetric entanglement can cancel the exchangemore » effects. - Highlights: • Kapitza–Dirac diffraction of entangled particles shows multiparticle interference. • There is a discontinuity in the set of joint detection patterns of entangled states. • We find a complementary behavior between overlapping and Schmidt’s number. • Symmetric entanglement can cancel the exchange effects.« less

Understanding deformation with high angular resolution electron backscatter diffraction (HR-EBSD)

NASA Astrophysics Data System (ADS)

Britton, T. B.; Hickey, J. L. R.

2018-01-01

High angular resolution electron backscatter diffraction (HR-EBSD) affords an increase in angular resolution, as compared to ‘conventional’ Hough transform based EBSD, of two orders of magnitude, enabling measurements of relative misorientations of 1 x 10-4 rads (~ 0.006°) and changes in (deviatoric) lattice strain with a precision of 1 x 10-4. This is achieved through direct comparison of two or more diffraction patterns using sophisticated cross-correlation based image analysis routines. Image shifts between zone axes in the two-correlated diffraction pattern are measured with sub-pixel precision and this realises the ability to measure changes in interplanar angles and lattice orientation with a high degree of sensitivity. These shifts are linked to strains and lattice rotations through simple geometry. In this manuscript, we outline the basis of the technique and two case studies that highlight its potential to tackle real materials science challenges, such as deformation patterning in polycrystalline alloys.

Sub-diffraction limit laser ablation via multiple exposures using a digital micromirror device.

PubMed

Heath, Daniel J; Grant-Jacob, James A; Feinaeugle, Matthias; Mills, Ben; Eason, Robert W

2017-08-01

We present the use of digital micromirror devices as variable illumination masks for pitch-splitting multiple exposures to laser machine the surfaces of materials. Ultrafast laser pulses of length 150 fs and 800 nm central wavelength were used for the sequential machining of contiguous patterns on the surface of samples in order to build up complex structures with sub-diffraction limit features. Machined patterns of tens to hundreds of micrometers in lateral dimensions with feature separations as low as 270 nm were produced in electroless nickel on an optical setup diffraction limited to 727 nm, showing a reduction factor below the Abbe diffraction limit of ∼2.7×. This was compared to similar patterns in a photoresist optimized for two-photon absorption, which showed a reduction factor of only 2×, demonstrating that multiple exposures via ablation can produce a greater resolution enhancement than via two-photon polymerization.

Two-Dimensional Light Diffraction from an EPROM Chip

ERIC Educational Resources Information Center

Ekkens, Tom

2018-01-01

In introductory physics classes, a laser pointer and a compact disc are all the items required to illustrate diffraction of light in a single dimension. If a two-dimensional diffraction pattern is desired, double axis diffraction grating material is available or a CCD sensor can be extracted from an unused electronics device. This article presents…

Local and average structures of BaTiO 3-Bi(Zn 1/2Ti 1/2)O 3

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

Usher, Tedi-Marie; Iamsasri, Thanakorn; Forrester, Jennifer S.

The complex crystallographic structures of (1-x)BaTiO 3-xBi(Zn 1/2Ti 1/2)O 3 (BT-xBZT) are examined using high resolution synchrotron X-ray diffraction, neutron diffraction, and neutron pair distribution function (PDF) analyses. The short-range structures are characterized from the PDFs, and a combined analysis of the X-ray and neutron diffraction patterns is used to determine the long-range structures. Our results demonstrate that the structure appears different when averaged over different length scales. In all compositions, the local structures determined from the PDFs show local tetragonal distortions (i.e., c/a > 1). But, a box-car fitting analysis of the PDFs reveals variations at different length scales.more » For 0.80BT-0.20BZT and 0.90BT-0.10BZT, the tetragonal distortions decrease at longer atom-atom distances (e.g., 30 vs. 5 ). When the longest distances are evaluated (r > 40 ), the lattice parameters approach cubic. Neutron and X-ray diffraction yield further information about the long-range structure. Compositions 0.80BT-0.20BZT and 0.90BT-0.10BZT appear cubic by Bragg diffraction (no peak splitting), consistent with the PDFs at long distances. However, these patterns cannot be adequately fit using a cubic lattice model; modeling their structures with the P4mm space group allows for a better fit to the patterns because the space group allows for c-axis atomic displacements that occur at the local scale. Furthermore, for the compositions 0.92BT-0.08BZT and 0.94BT-0.06BZT, strong tetragonal distortions are observed at the local scale and a less-distorted tetragonal structure is observed at longer length scales. In Rietveld refinements, the latter is modeled using a tetragonal phase. Since the peak overlap in these two-phase compositions limits the ability to model the local-scale structures as tetragonal, it is approximated in the refinements as a cubic phase. These results demonstrate that alloying BT with BZT results in increased disorder and disrupts the long-range ferroelectric symmetry present in BT, while the large tetragonal distortion present in BZT persists at the local scale.« less

Local and average structures of BaTiO 3-Bi(Zn 1/2Ti 1/2)O 3

DOE PAGES

Usher, Tedi-Marie; Iamsasri, Thanakorn; Forrester, Jennifer S.; ...

2016-11-11

The complex crystallographic structures of (1-x)BaTiO 3-xBi(Zn 1/2Ti 1/2)O 3 (BT-xBZT) are examined using high resolution synchrotron X-ray diffraction, neutron diffraction, and neutron pair distribution function (PDF) analyses. The short-range structures are characterized from the PDFs, and a combined analysis of the X-ray and neutron diffraction patterns is used to determine the long-range structures. Our results demonstrate that the structure appears different when averaged over different length scales. In all compositions, the local structures determined from the PDFs show local tetragonal distortions (i.e., c/a > 1). But, a box-car fitting analysis of the PDFs reveals variations at different length scales.more » For 0.80BT-0.20BZT and 0.90BT-0.10BZT, the tetragonal distortions decrease at longer atom-atom distances (e.g., 30 vs. 5 ). When the longest distances are evaluated (r > 40 ), the lattice parameters approach cubic. Neutron and X-ray diffraction yield further information about the long-range structure. Compositions 0.80BT-0.20BZT and 0.90BT-0.10BZT appear cubic by Bragg diffraction (no peak splitting), consistent with the PDFs at long distances. However, these patterns cannot be adequately fit using a cubic lattice model; modeling their structures with the P4mm space group allows for a better fit to the patterns because the space group allows for c-axis atomic displacements that occur at the local scale. Furthermore, for the compositions 0.92BT-0.08BZT and 0.94BT-0.06BZT, strong tetragonal distortions are observed at the local scale and a less-distorted tetragonal structure is observed at longer length scales. In Rietveld refinements, the latter is modeled using a tetragonal phase. Since the peak overlap in these two-phase compositions limits the ability to model the local-scale structures as tetragonal, it is approximated in the refinements as a cubic phase. These results demonstrate that alloying BT with BZT results in increased disorder and disrupts the long-range ferroelectric symmetry present in BT, while the large tetragonal distortion present in BZT persists at the local scale.« less

Single-particle structure determination by correlations of snapshot X-ray diffraction patterns (CXIDB ID 20)

DOE Data Explorer

Starodub, D.

2013-03-25

This deposition includes the diffraction images generated by the paired polystyrene spheres in random orientations. These images were used to determine and phase the single particle diffraction volume from their autocorrelation functions.

A compact electron gun for time-resolved electron diffraction

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

Robinson, Matthew S.; Lane, Paul D.; Wann, Derek A., E-mail: derek.wann@york.ac.uk

A novel compact time-resolved electron diffractometer has been built with the primary goal of studying the ultrafast molecular dynamics of photoexcited gas-phase molecules. Here, we discuss the design of the electron gun, which is triggered by a Ti:Sapphire laser, before detailing a series of calibration experiments relating to the electron-beam properties. As a further test of the apparatus, initial diffraction patterns have been collected for thin, polycrystalline platinum samples, which have been shown to match theoretical patterns. The data collected demonstrate the focusing effects of the magnetic lens on the electron beam, and how this relates to the spatial resolutionmore » of the diffraction pattern.« less

Disentangling atomic-layer-specific x-ray absorption spectra by Auger electron diffraction spectroscopy

NASA Astrophysics Data System (ADS)

Matsui, Fumihiko; Matsushita, Tomohiro; Kato, Yukako; Hashimoto, Mie; Daimon, Hiroshi

2009-11-01

In order to investigate the electronic and magnetic structures of each atomic layer at subsurface, we have proposed a new method, Auger electron diffraction spectroscopy, which is the combination of x-ray absorption spectroscopy (XAS) and Auger electron diffraction (AED) techniques. We have measured a series of Ni LMM AED patterns of the Ni film grown on Cu(001) surface for various thicknesses. Then we deduced a set of atomic-layer-specific AED patterns in a numerical way. Furthermore, we developed an algorithm to disentangle XANES spectra from different atomic layers using these atomic-layer-specific AED patterns. Surface and subsurface core level shift were determined for each atomic layer.

Tests of Si(111)-7 × 7 structural models by comparison with transmission electron diffraction patterns

NASA Astrophysics Data System (ADS)

McRae, E. G.; Petroff, P. M.

1984-11-01

Several structural models of the Si(111)-7 × 7 surface are tested by comparing calculated and observed transmission electron diffraction (TED) patterns. The models comprise "adatom" models where the unit mesh contains 12 adatoms or atom clusters in a locally (2 × 2) arrangement, and "triangle-dimer" models where the unit mesh contains 9 dimers or pairs of dimers bordering a triangular subunit of the unit mesh. The distribution of diffraction intensity among fractional-order spots is calculated kinematically and compared with TED patterns observed by Petroff and Wilson and others. No agreement is found for adatom models. Good but not perfect agreement is found for one triangle-dimer model.

Evaluating diffraction based overlay metrology for double patterning technologies

NASA Astrophysics Data System (ADS)

Saravanan, Chandra Saru; Liu, Yongdong; Dasari, Prasad; Kritsun, Oleg; Volkman, Catherine; Acheta, Alden; La Fontaine, Bruno

2008-03-01

Demanding sub-45 nm node lithographic methodologies such as double patterning (DPT) pose significant challenges for overlay metrology. In this paper, we investigate scatterometry methods as an alternative approach to meet these stringent new metrology requirements. We used a spectroscopic diffraction-based overlay (DBO) measurement technique in which registration errors are extracted from specially designed diffraction targets for double patterning. The results of overlay measurements are compared to traditional bar-in-bar targets. A comparison between DBO measurements and CD-SEM measurements is done to show the correlation between the two approaches. We discuss the total measurement uncertainty (TMU) requirements for sub-45 nm nodes and compare TMU from the different overlay approaches.

Synthesis and characterization of nanoparticles conjugated tannase and using it for enhancement of antibacterial activity of tannase produced by Serratia marcescens.

PubMed

Nsayef Muslim, D Sahira; Abbas Dham, Ziyad; J Mohammed, D Nadheer

2017-09-01

Fourteen isolates of Serratia marcescens were collected from patients suffering from septicemia. All theseisolates revealed different levels in tannase production. Tannase was partially purified from Serratia marcescens b9 by precipitation method at 70% saturation of ammonium sulfate. Au, Pt, SnO 2 and SiO 2 nanoparticles were prepared by laser ablation and examined by transmission electron microscopy (TEM), X-ray diffraction pattern and UV-Visible absorption spectroscopy. Conjugation of SiO 2 nanoparticles to tannase by feeding and pulses methods were prepared and characterized by TEM, X-ray diffraction pattern and UV-Visible spectrum. SiO 2 nanoparticles conjugated partially purified tannase by feeding showed the higher effectiveness and higher significant level against all tested UTI causing in comparison with ciprofloxacin antibiotic, SiO 2 nanoparticles alone, partially purified tannase alone and partially purified tannase by pulses. So that we can conclude that feeding method was the best method for enhancement partially purified tannase activity to maximum level thus SiO 2 nanoparticles conjugated partially purified tannase may be a useful antibacterial agent for the treatment of urinary tract infection. Copyright © 2017 Elsevier Ltd. All rights reserved.

Incorrect support and missing center tolerances of phasing algorithms

DOE PAGES

Huang, Xiaojing; Nelson, Johanna; Steinbrener, Jan; ...

2010-01-01

In x-ray diffraction microscopy, iterative algorithms retrieve reciprocal space phase information, and a real space image, from an object's coherent diffraction intensities through the use of a priori information such as a finite support constraint. In many experiments, the object's shape or support is not well known, and the diffraction pattern is incompletely measured. We describe here computer simulations to look at the effects of both of these possible errors when using several common reconstruction algorithms. Overly tight object supports prevent successful convergence; however, we show that this can often be recognized through pathological behavior of the phase retrieval transfermore » function. Dynamic range limitations often make it difficult to record the central speckles of the diffraction pattern. We show that this leads to increasing artifacts in the image when the number of missing central speckles exceeds about 10, and that the removal of unconstrained modes from the reconstructed image is helpful only when the number of missing central speckles is less than about 50. In conclusion, this simulation study helps in judging the reconstructability of experimentally recorded coherent diffraction patterns.« less

Single beam write and/or replay of spatial heterodyne holograms

DOEpatents

Thomas, Clarence E.; Hanson, Gregory R.

2007-11-20

A method of writing a spatially heterodyne hologram having spatially heterodyne fringes includes: passing a single write beam through a spatial light modulator that digitally modulates said single write beam; and focusing the single write beam at a focal plane of a lens to impose a holographic diffraction grating pattern on the photorefractive crystal, the holographic diffraction grating pattern including the spatially heterodyne hologram having spatially heterodyne fringes, wherein only said single write beam is incident on said photorefractive crystal without a reference beam. A method of replaying a spatially heterodyne hologram having spatially heterodyne fringes at a replay angle includes: illuminating a photorefractive crystal having a holographic diffraction grating with a beam from a laser at an illumination angle, the holographic diffraction grating pattern including the spatially heterodyne hologram having spatially heterodyne fringes, wherein a difference between said illumination angle and said replay angle defines a diffraction angle .alpha. that is a function of a plane wave mathematically added to original object wave phase and amplitude data of said spatially heterodyne hologram having spatially heterodyne fringes.

Detecting diffusion-diffraction patterns in size distribution phantoms using double-pulsed field gradient NMR: Theory and experiments.

PubMed

Shemesh, Noam; Ozarslan, Evren; Basser, Peter J; Cohen, Yoram

2010-01-21

NMR observable nuclei undergoing restricted diffusion within confining pores are important reporters for microstructural features of porous media including, inter-alia, biological tissues, emulsions and rocks. Diffusion NMR, and especially the single-pulsed field gradient (s-PFG) methodology, is one of the most important noninvasive tools for studying such opaque samples, enabling extraction of important microstructural information from diffusion-diffraction phenomena. However, when the pores are not monodisperse and are characterized by a size distribution, the diffusion-diffraction patterns disappear from the signal decay, and the relevant microstructural information is mostly lost. A recent theoretical study predicted that the diffusion-diffraction patterns in double-PFG (d-PFG) experiments have unique characteristics, such as zero-crossings, that make them more robust with respect to size distributions. In this study, we theoretically compared the signal decay arising from diffusion in isolated cylindrical pores characterized by lognormal size distributions in both s-PFG and d-PFG methodologies using a recently presented general framework for treating diffusion in NMR experiments. We showed the gradual loss of diffusion-diffraction patterns in broadening size distributions in s-PFG and the robustness of the zero-crossings in d-PFG even for very large standard deviations of the size distribution. We then performed s-PFG and d-PFG experiments on well-controlled size distribution phantoms in which the ground-truth is well-known a priori. We showed that the microstructural information, as manifested in the diffusion-diffraction patterns, is lost in the s-PFG experiments, whereas in d-PFG experiments the zero-crossings of the signal persist from which relevant microstructural information can be extracted. This study provides a proof of concept that d-PFG may be useful in obtaining important microstructural features in samples characterized by size distributions.

Measuring Three-Dimensional Strain and Structural Defects in a Single InGaAs Nanowire Using Coherent X-ray Multiangle Bragg Projection Ptychography

DOE PAGES

Hill, Megan O.; Calvo-Almazan, Irene; Allain, Marc; ...

2018-01-08

III - As nanowires are candidates for near-infrared light emitters and detectors that can be directly integrated onto silicon. However, nanoscale to microscale variations in structure, composition, and strain within a given nanowire, as well as variations between nanowires, pose challenges to correlating microstructure with device performance. In this work, we utilize coherent nanofocused X-rays to characterize stacking defects and strain in a single InGaAs nanowire supported on Si. By reconstructing diffraction patterns from the 2110 Bragg peak, we show that the lattice orientation varies along the length of the wire, while the strain field along the cross-section is largelymore » unaffected, leaving the band structure unperturbed. Diffraction patterns from the 0110 Bragg peak are reproducibly reconstructed to create three-dimensional images of stacking defects and associated lattice strains, revealing sharp planar boundaries between different crystal phases of wurtzite (WZ) structure that contribute to charge carrier scattering. Phase retrieval is made possible by developing multiangle Bragg projection ptychography (maBPP) to accommodate coherent nanodiffraction patterns measured at arbitrary overlapping positions at multiple angles about a Bragg peak, eliminating the need for scan registration at different angles. The penetrating nature of X-ray radiation, together with the relaxed constraints of maBPP, will enable the in operando imaging of nanowire devices.« less

Measuring Three-Dimensional Strain and Structural Defects in a Single InGaAs Nanowire Using Coherent X-ray Multiangle Bragg Projection Ptychography

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

Hill, Megan O.; Calvo-Almazan, Irene; Allain, Marc

III - As nanowires are candidates for near-infrared light emitters and detectors that can be directly integrated onto silicon. However, nanoscale to microscale variations in structure, composition, and strain within a given nanowire, as well as variations between nanowires, pose challenges to correlating microstructure with device performance. In this work, we utilize coherent nanofocused X-rays to characterize stacking defects and strain in a single InGaAs nanowire supported on Si. By reconstructing diffraction patterns from the 2110 Bragg peak, we show that the lattice orientation varies along the length of the wire, while the strain field along the cross-section is largelymore » unaffected, leaving the band structure unperturbed. Diffraction patterns from the 0110 Bragg peak are reproducibly reconstructed to create three-dimensional images of stacking defects and associated lattice strains, revealing sharp planar boundaries between different crystal phases of wurtzite (WZ) structure that contribute to charge carrier scattering. Phase retrieval is made possible by developing multiangle Bragg projection ptychography (maBPP) to accommodate coherent nanodiffraction patterns measured at arbitrary overlapping positions at multiple angles about a Bragg peak, eliminating the need for scan registration at different angles. The penetrating nature of X-ray radiation, together with the relaxed constraints of maBPP, will enable the in operando imaging of nanowire devices.« less

Cancer cell classification with coherent diffraction imaging using an extreme ultraviolet radiation source

PubMed Central

Zürch, Michael; Foertsch, Stefan; Matzas, Mark; Pachmann, Katharina; Kuth, Rainer; Spielmann, Christian

2014-01-01

Abstract. In cancer treatment, it is highly desirable to classify single cancer cells in real time. The standard method is polymerase chain reaction requiring a substantial amount of resources and time. Here, we present an innovative approach for rapidly classifying different cell types: we measure the diffraction pattern of a single cell illuminated with coherent extreme ultraviolet (XUV) laser-generated radiation. These patterns allow distinguishing different breast cancer cell types in a subsequent step. Moreover, the morphology of the object can be retrieved from the diffraction pattern with submicron resolution. In a proof-of-principle experiment, we prepared single MCF7 and SKBR3 breast cancer cells on gold-coated silica slides. The output of a laser-driven XUV light source is focused onto a single unstained and unlabeled cancer cell. With the resulting diffraction pattern, we could clearly identify the different cell types. With an improved setup, it will not only be feasible to classify circulating tumor cells with a high throughput, but also to identify smaller objects such as bacteria or even viruses. PMID:26158049

Cancer cell classification with coherent diffraction imaging using an extreme ultraviolet radiation source.

PubMed

Zürch, Michael; Foertsch, Stefan; Matzas, Mark; Pachmann, Katharina; Kuth, Rainer; Spielmann, Christian

2014-10-01

In cancer treatment, it is highly desirable to classify single cancer cells in real time. The standard method is polymerase chain reaction requiring a substantial amount of resources and time. Here, we present an innovative approach for rapidly classifying different cell types: we measure the diffraction pattern of a single cell illuminated with coherent extreme ultraviolet (XUV) laser-generated radiation. These patterns allow distinguishing different breast cancer cell types in a subsequent step. Moreover, the morphology of the object can be retrieved from the diffraction pattern with submicron resolution. In a proof-of-principle experiment, we prepared single MCF7 and SKBR3 breast cancer cells on gold-coated silica slides. The output of a laser-driven XUV light source is focused onto a single unstained and unlabeled cancer cell. With the resulting diffraction pattern, we could clearly identify the different cell types. With an improved setup, it will not only be feasible to classify circulating tumor cells with a high throughput, but also to identify smaller objects such as bacteria or even viruses.

Evaluation of Argon ion irradiation hardening of ferritic/martensitic steel-T91 using nanoindentation, X-ray diffraction and TEM techniques

NASA Astrophysics Data System (ADS)

Naveen Kumar, N.; Tewari, R.; Mukherjee, P.; Gayathri, N.; Durgaprasad, P. V.; Taki, G. S.; Krishna, J. B. M.; Sinha, A. K.; Pant, P.; Revally, A. K.; Dutta, B. K.; Dey, G. K.

2017-08-01

In the present study, microstructures of Ferritic-martensitic T-91 steel irradiated at room temperature for 5, 10 and 20 dpa using 315 KeV Ar+9 ions have been characterized by grazing incident X-ray diffraction (GIXRD) and by transmission electron microscopy (TEM). Line profiles of GIXRD patterns have shown that the size of domain continuously reduced with increasing dose of radiation. TEM investigations of irradiated samples have shown the presence of black dots, the number density of which decreases with increasing dose. Microstructures of irradiated samples have also revealed the presence of point defect clusters, such as dislocation loops and bubbles. In addition, dissolution of precipitates due to irradiation was also observed. Nano-indentation studies on the irradiated samples have shown saturation behavior in hardness as a function of dose which could be correlated with the changes in the yield strength of the alloy.

Anodic Aluminum Oxide Membrane-Assisted Fabrication of beta-In(2)S(3) Nanowires.

PubMed

Shi, Jen-Bin; Chen, Chih-Jung; Lin, Ya-Ting; Hsu, Wen-Chia; Chen, Yu-Cheng; Wu, Po-Feng

2009-06-06

In this study, beta-In(2)S(3) nanowires were first synthesized by sulfurizing the pure Indium (In) nanowires in an AAO membrane. As FE-SEM results, beta-In(2)S(3) nanowires are highly ordered, arranged tightly corresponding to the high porosity of the AAO membrane used. The diameter of the beta-In(2)S(3) nanowires is about 60 nm with the length of about 6-8 mum. Moreover, the aspect ratio of beta-In(2)S(3) nanowires is up to 117. An EDS analysis revealed the beta-In(2)S(3) nanowires with an atomic ratio of nearly S/In = 1.5. X-ray diffraction and corresponding selected area electron diffraction patterns demonstrated that the beta-In(2)S(3) nanowire is tetragonal polycrystalline. The direct band gap energy (E(g)) is 2.40 eV from the optical measurement, and it is reasonable with literature.

Crystal structure, spectrum character and explosive property of a new cocrystal CL-20/DNT

NASA Astrophysics Data System (ADS)

Liu, Ke; Zhang, Gao; Luan, Jieyu; Chen, Zhiqun; Su, Pengfei; Shu, Yuanjie

2016-04-01

A new cocrystal explosive of 2,4,6,8,10,12-hexanitrohexaazaiso-wurtzitane(CL-20) and 2,5-dinitrotoluene(DNT) in a molar ratio of 1:2 has been prepared by slow solvent evaporation method. Crystal structure of the cocrystal characterized by single crystal X-ray diffraction (SXRD) reveals that the cocrystal is formed by intermolecular hydrogen bond interactions and belongs to the triclinic system with P-1 group. Moreover, the obivious differences of powder X-ray diffraction (PXRD) patterns, infrared spectroscopy and Raman spectroscopy confirm that the intermolecular interactions have great influence for the crystal structure and formation of cocrystal. The cocrystal exhibits a lower impact height of 44 cm, suggesting a substantial reduction of sensitivity in comparison with CL-20. And thermal test results showed cocrystal obtains a lower melting point than DNT, which means huge advantages in blasting engineering.

Utilizing boron nitride sheets as thin supports for high resolution imaging of nanocrystals.

PubMed

Wu, Yimin A; Kirkland, Angus I; Schäffel, Franziska; Porfyrakis, Kyriakos; Young, Neil P; Briggs, G Andrew D; Warner, Jamie H

2011-05-13

We demonstrate the use of thin BN sheets as supports for imaging nanocrystals using low voltage (80 kV) aberration-corrected high resolution transmission electron microscopy. This provides an alternative to the previously utilized 2D crystal supports of graphene and graphene oxide. A simple chemical exfoliation method is applied to get few layer boron nitride (BN) sheets with micrometer-sized dimensions. This generic approach of using BN sheets as supports is shown by depositing Mn doped ZnSe nanocrystals directly onto the BN sheets and resolving the atomic structure from both the ZnSe nanocrystals and the BN support. Phase contrast images reveal moiré patterns of interference between the beams diffracted by the nanocrystals and the BN substrate that are used to determine the relative orientation of the nanocrystals with respect to the BN sheets and interference lattice planes. Double diffraction is observed and has been analyzed.

Room Temperature Gas Sensing Properties of Sn-Substituted Nickel Ferrite (NiFe2O4) Thin Film Sensors Prepared by Chemical Co-Precipitation Method

NASA Astrophysics Data System (ADS)

Manikandan, V.; Li, Xiaogan; Mane, R. S.; Chandrasekaran, J.

2018-04-01

Tin (Sn) substituted nickel ferrite (NiFe2O4) thin film sensors were prepared by a simple chemical co-precipitation method, which initially characterized their structure and surface morphology with the help of x-ray diffraction and scanning electron microscopy. Surface morphology of the sensing films reveals particles stick together with nearer particles and this formation leads to a large specific area as a large specific area is very useful for easy adsorption of gas molecules. Transmission electron microscopy and selected area electron diffraction pattern images confirm particle size and nanocrystallnity as due to formation of circular rings. Fourier transform infrared analysis has supported the presence of functional groups. The 3.69 eV optical band gap of the film was found which enabled better gas sensing. Gas sensors demonstrate better response and recovery characteristics, and the maximum response was 68.43%.

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

Marimuthu, T.; Anandhan, N., E-mail: anandhan-kn@rediffmail.com; Mummoorthi, M.

Zinc oxide (ZnO) and zinc oxide/eosin yellow (ZnO/EY) thin films were potentiostatically deposited onto fluorine doped tin oxide (FTO) glass substrate. Effect of eosin yellow dye on structural, morphological and optical properties was studied. X-ray diffraction patterns, micro Raman spectra and photoluminescence (PL) spectra reveal hexagonal wurtzite structure with less atomic defects in 101 plane orientation of the ZnO/EY film. Scanning electron microscopy (SEM) images show flower for ZnO and porous like structure for ZnO/EY thin film, respectively. DSSC was constructed and evaluated by measuring the current density verses voltage curve.

Surprising synthesis of nanodiamond from single-walled carbon nanotubes by the spark plasma sintering process

NASA Astrophysics Data System (ADS)

Mirzaei, Ali; Ham, Heon; Na, Han Gil; Kwon, Yong Jung; Kang, Sung Yong; Choi, Myung Sik; Bang, Jae Hoon; Park, No-Hyung; Kang, Inpil; Kim, Hyoun Woo

2016-10-01

Nanodiamond (ND) was successfully synthesized using single-walled carbon nanotubes (SWCNTs) as a pure solid carbon source by means of a spark plasma sintering process. Raman spectra and X-ray diffraction patterns revealed the generation of the cubic diamond phase by means of the SPS process. Lattice-resolved TEM images confirmed that diamond nanoparticles with a diameter of about ˜10 nm existed in the products. The NDs were generated mainly through the gas-phase nucleation of carbon atoms evaporated from the SWCNTs. [Figure not available: see fulltext.

Structural, optical and AFM characterization of PVA:La3+ polymer films

NASA Astrophysics Data System (ADS)

Ali, F. M.; Maiz, F.

2018-02-01

In this paper the structural and optical properties of pure Polyvinyl alcohol (PVA) and La3+-doped PVA films in the concentration range of 4%, 12% and 20% weight percent of Lanthanum were prepared by the conventional casting technique. X-ray diffraction pattern and atomic force microscopy studies of the investigated samples reveal their semi-crystalline nature. It is found that, absorption coefficient and cluster size of lanthanum:PVA composite increase with increasing salt concentration. However, the optical energy gap shows a slight decreasing trend.

Fast computation algorithms for speckle pattern simulation

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

Nascov, Victor; Samoilă, Cornel; Ursuţiu, Doru

2013-11-13

We present our development of a series of efficient computation algorithms, generally usable to calculate light diffraction and particularly for speckle pattern simulation. We use mainly the scalar diffraction theory in the form of Rayleigh-Sommerfeld diffraction formula and its Fresnel approximation. Our algorithms are based on a special form of the convolution theorem and the Fast Fourier Transform. They are able to evaluate the diffraction formula much faster than by direct computation and we have circumvented the restrictions regarding the relative sizes of the input and output domains, met on commonly used procedures. Moreover, the input and output planes canmore » be tilted each to other and the output domain can be off-axis shifted.« less

Macromolecular diffractive imaging using imperfect crystals

PubMed Central

Ayyer, Kartik; Yefanov, Oleksandr; Oberthür, Dominik; Roy-Chowdhury, Shatabdi; Galli, Lorenzo; Mariani, Valerio; Basu, Shibom; Coe, Jesse; Conrad, Chelsie E.; Fromme, Raimund; Schaffer, Alexander; Dörner, Katerina; James, Daniel; Kupitz, Christopher; Metz, Markus; Nelson, Garrett; Lourdu Xavier, Paulraj; Beyerlein, Kenneth R.; Schmidt, Marius; Sarrou, Iosifina; Spence, John C. H.; Weierstall, Uwe; White, Thomas A.; Yang, Jay-How; Zhao, Yun; Liang, Mengning; Aquila, Andrew; Hunter, Mark S.; Robinson, Joseph S.; Koglin, Jason E.; Boutet, Sébastien; Fromme, Petra; Barty, Anton; Chapman, Henry N.

2016-01-01

The three-dimensional structures of macromolecules and their complexes are predominantly elucidated by X-ray protein crystallography. A major limitation is access to high-quality crystals, to ensure X-ray diffraction extends to sufficiently large scattering angles and hence yields sufficiently high-resolution information that the crystal structure can be solved. The observation that crystals with shrunken unit-cell volumes and tighter macromolecular packing often produce higher-resolution Bragg peaks1,2 hints that crystallographic resolution for some macromolecules may be limited not by their heterogeneity but rather by a deviation of strict positional ordering of the crystalline lattice. Such displacements of molecules from the ideal lattice give rise to a continuous diffraction pattern, equal to the incoherent sum of diffraction from rigid single molecular complexes aligned along several discrete crystallographic orientations and hence with an increased information content3. Although such continuous diffraction patterns have long been observed—and are of interest as a source of information about the dynamics of proteins4 —they have not been used for structure determination. Here we show for crystals of the integral membrane protein complex photosystem II that lattice disorder increases the information content and the resolution of the diffraction pattern well beyond the 4.5 Å limit of measurable Bragg peaks, which allows us to directly phase5 the pattern. With the molecular envelope conventionally determined at 4.5 Å as a constraint, we then obtain a static image of the photosystem II dimer at 3.5 Å resolution. This result shows that continuous diffraction can be used to overcome long-supposed resolution limits of macromolecular crystallography, with a method that puts great value in commonly encountered imperfect crystals and opens up the possibility for model-free phasing6,7. PMID:26863980

Data preparation and evaluation techniques for x-ray diffraction microscopy.

PubMed

Steinbrener, Jan; Nelson, Johanna; Huang, Xiaojing; Marchesini, Stefano; Shapiro, David; Turner, Joshua J; Jacobsen, Chris

2010-08-30

The post-experiment processing of X-ray Diffraction Microscopy data is often time-consuming and difficult. This is mostly due to the fact that even if a preliminary result has been reconstructed, there is no definitive answer as to whether or not a better result with more consistently retrieved phases can still be obtained. We show here that the first step in data analysis, the assembly of two-dimensional diffraction patterns from a large set of raw diffraction data, is crucial to obtaining reconstructions of highest possible consistency. We have developed software that automates this process and results in consistently accurate diffraction patterns. We have furthermore derived some criteria of validity for a tool commonly used to assess the consistency of reconstructions, the phase retrieval transfer function, and suggest a modified version that has improved utility for judging reconstruction quality.

Diffraction experiments with infrared remote controls

NASA Astrophysics Data System (ADS)

Kuhn, Jochen; Vogt, Patrik

2012-02-01

In this paper we describe an experiment in which radiation emitted by an infrared remote control is passed through a diffraction grating. An image of the diffraction pattern is captured using a cell phone camera and then used to determine the wavelength of the radiation.

Method to mosaic gratings that relies on analysis of far-field intensity patterns in two wavelengths

NASA Astrophysics Data System (ADS)

Hu, Yao; Zeng, Lijiang; Li, Lifeng

2007-01-01

We propose an experimental method to coherently mosaic two planar diffraction gratings. The method uses a Twyman-Green interferometer to guarantee the planar parallelism of the two sub-aperture gratings, and obtains the in-plane rotational error and the two translational errors from analysis of the far-field diffraction intensity patterns in two alignment wavelengths. We adjust the relative attitude and position of the two sub-aperture gratings to produce Airy disk diffraction patterns in both wavelengths. In our experiment, the repeatability of in-plane rotation adjustment was 2.35 μrad and that of longitudinal adjustment was 0.11 μm. The accuracy of lateral adjustment was about 2.9% of the grating period.

Mechanical diffraction in a sand-specialist snake

NASA Astrophysics Data System (ADS)

Schiebel, Perrin E.; Rieser, Jennifer M.; Hubbard, Alex M.; Chen, Lillian; Goldman, Daniel I.

Limbless locomotors such as snakes move by pressing the trunk against terrain heterogeneities. Our laboratory studies of the desert-dwelling Mojave Shovel-nosed snake (C. occipitalis, 40cm long, N=9) reveal that these animals use a stereotyped sinusoidal traveling wave of curvature. However, this snake also encounters rigid obstacles in its natural environment, and the tradeoff between using a cyclic, shape controlled gait versus one which changes shape in response to the terrain is not well understood. We challenged individuals to move across a model deformable substrate (carpet) through a row of 6.4 mm diameter force-sensitive pegs, a model of obstacles such as grass, oriented perpendicular to the direction of motion. Instead of forward-directed reaction forces, reaction forces generated by the pegs were more often perpendicular to the direction of motion. Distributions of post-peg travel angles displayed preferred directions revealing a diffraction-like pattern with a central peak at zero and symmetric peaks at 193 ° and 415 °. We observed similar dynamics in a robotic snake using shape-based control. This suggests that this sand-specialist snake adheres to its preferred waveform as opposed to changing in response to heterogeneity.

Kirigami Nanocomposites as Wide-Angle Diffraction Gratings.

PubMed

Xu, Lizhi; Wang, Xinzhi; Kim, Yoonseob; Shyu, Terry C; Lyu, Jing; Kotov, Nicholas A

2016-06-28

Beam steering devices represent an essential part of an advanced optics toolbox and are needed in a spectrum of technologies ranging from astronomy and agriculture to biosensing and networked vehicles. Diffraction gratings with strain-tunable periodicity simplify beam steering and can serve as a foundation for light/laser radar (LIDAR/LADAR) components of robotic systems. However, the mechanical properties of traditional materials severely limit the beam steering angle and cycle life. The large strain applied to gratings can severely impair the device performance both in respect of longevity and diffraction pattern fidelity. Here, we show that this problem can be resolved using micromanufactured kirigami patterns from thin film nanocomposites based on high-performance stiff plastics, metals, and carbon nanotubes, etc. The kirigami pattern of microscale slits reduces the stochastic concentration of strain in stiff nanocomposites including those made by layer-by-layer assembly (LBL). The slit patterning affords reduction of strain by 2 orders of magnitude for stretching deformation and consequently enables reconfigurable optical gratings with over a 100% range of period tunability. Elasticity of the stiff nanocomposites and plastics makes possible cyclic reconfigurability of the grating with variable time constant that can also be referred to as 4D kirigami. High-contrast, sophisticated diffraction patterns with as high as fifth diffraction order can be obtained. The angular range of beam steering can be as large as 6.5° for a 635 nm laser beam compared to ∼1° in surface-grooved elastomer gratings and ∼0.02° in MEMS gratings. The versatility of the kirigami patterns, the diversity of the available nanocomposite materials, and their advantageous mechanical properties of the foundational materials open the path for engineering of reconfigurable optical elements in LIDARs essential for autonomous vehicles and other optical devices with spectral range determined by the kirigami periodicity.

Preparation of PVA/Co/Ag film and evaluation of its magnetic and microstructural properties

NASA Astrophysics Data System (ADS)

Banerjee, M.; Sachdev, Preeti; Mukherjee, G. S.

2012-05-01

PVA/Co/Ag film has been prepared by sputtering Co followed by Ag in polyvinyl alcohol (PVA) matrix film by IBS technique, so as to get a 9 nm (thick) layer of Co metal nanoparticles followed by a protective 4 nm (thick) layer of Ag nanoparticles. Grazing incidence x-ray diffraction (GIXRD) pattern of the film reveals the formation of nanocrystalline Co with hcp phase. GIXRD pattern also indicates that there is no change in the crystalline structure of PVA even after sputtering of the metallic nanoparticles. The average particle size of Co nanoparticles as evaluated using Scherrer formula is found to be about 2.64 nm. UV visible absorption pattern of the film sample showed SPR peaks of Co and Ag metals in their nano size level embedded in the PVA matrix system. XPS study confirms the metallic nature of Co and Ag nanoparticles; and the depth profiling study reveals that both the metal nanoparticles have been embedded in the PVA matrix system. Surface morphology of such film has been studied using AFM; and the magnetic behaviour of the film studied by using MOKE shows soft ferromagnetic behaviour in this PVA/Co/Ag system.

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.

Theoretical study of the properties of X-ray diffraction moiré fringes. I

PubMed Central

Yoshimura, Jun-ichi

2015-01-01

A detailed and comprehensive theoretical description of X-ray diffraction moiré fringes for a bicrystal specimen is given on the basis of a calculation by plane-wave dynamical diffraction theory. Firstly, prior to discussing the main subject of the paper, a previous article [Yoshimura (1997 ▸). Acta Cryst. A53, 810–812] on the two-dimensionality of diffraction moiré patterns is restated on a thorough calculation of the moiré interference phase. Then, the properties of moiré fringes derived from the above theory are explained for the case of a plane-wave diffraction image, where the significant effect of Pendellösung intensity oscillation on the moiré pattern when the crystal is strained is described in detail with theoretically simulated moiré images. Although such plane-wave moiré images are not widely observed in a nearly pure form, knowledge of their properties is essential for the understanding of diffraction moiré fringes in general. PMID:25970298

A Simple Diffraction Experiment Using Banana Stem as a Natural Grating

ERIC Educational Resources Information Center

Aji, Mahardika Prasetya; Karunawan, Jotti; Chasanah, Widyastuti Rochimatun; Nursuhud, Puji Iman; Wiguna, Pradita Ajeng; Sulhadi

2017-01-01

A simple diffraction experiment was designed using banana stem as natural grating. Coherent beams of lasers with wavelengths of 632.8 nm and 532 nm that pass through banana stem produce periodic diffraction patterns on a screen. The diffraction experiments were able to measure the distances between the slit of the banana stem, i.e. d = (28.76 ±…

Numerical comparison of grid pattern diffraction effects through measurement and modeling with OptiScan software

NASA Astrophysics Data System (ADS)

Murray, Ian B.; Densmore, Victor; Bora, Vaibhav; Pieratt, Matthew W.; Hibbard, Douglas L.; Milster, Tom D.

2011-06-01

Coatings of various metalized patterns are used for heating and electromagnetic interference (EMI) shielding applications. Previous work has focused on macro differences between different types of grids, and has shown good correlation between measurements and analyses of grid diffraction. To advance this work, we have utilized the University of Arizona's OptiScan software, which has been optimized for this application by using the Babinet Principle. When operating on an appropriate computer system, this algorithm produces results hundreds of times faster than standard Fourier-based methods, and allows realistic cases to be modeled for the first time. By using previously published derivations by Exotic Electro-Optics, we compare diffraction performance of repeating and randomized grid patterns with equivalent sheet resistance using numerical performance metrics. Grid patterns of each type are printed on optical substrates and measured energy is compared against modeled energy.

Exploring transmission Kikuchi diffraction using a Timepix detector

NASA Astrophysics Data System (ADS)

Vespucci, S.; Winkelmann, A.; Mingard, K.; Maneuski, D.; O'Shea, V.; Trager-Cowan, C.

2017-02-01

Electron backscatter diffraction (EBSD) is a well-established scanning electron microscope (SEM)-based technique [1]. It allows the non-destructive mapping of the crystal structure, texture, crystal phase and strain with a spatial resolution of tens of nanometers. Conventionally this is performed by placing an electron sensitive screen, typically consisting of a phosphor screen combined with a charge coupled device (CCD) camera, in front of a specimen, usually tilted 70° to the normal of the exciting electron beam. Recently, a number of authors have shown that a significant increase in spatial resolution is achievable when Kikuchi diffraction patterns are acquired in transmission geometry; that is when diffraction patterns are generated by electrons transmitted through an electron-transparent, usually thinned, specimen. The resolution of this technique, called transmission Kikuchi diffraction (TKD), has been demonstrated to be better than 10 nm [2,3]. We have recently demonstrated the advantages of a direct electron detector, Timepix [4,5], for the acquisition of standard EBSD patterns [5]. In this article we will discuss the advantages of Timepix to perform TKD and for acquiring spot diffraction patterns and more generally for acquiring scanning transmission electron microscopy micrographs in the SEM. Particularly relevant for TKD, is its very compact size, which allows much more flexibility in the positioning of the detector in the SEM chamber. We will furthermore show recent results using Timepix as a virtual forward scatter detector, and will illustrate the information derivable on producing images through processing of data acquired from different areas of the detector. We will show results from samples ranging from gold nanoparticles to nitride semiconductor nanorods.

High quality single shot ultrafast MeV electron diffraction from a photocathode radio-frequency gun

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

Fu, Feichao; Liu, Shengguang; Zhu, Pengfei

2014-08-15

A compact ultrafast electron diffractometer, consisting of an s-band 1.6 cell photocathode radio-frequency gun, a multi-function changeable sample chamber, and a sensitive relativistic electron detector, was built at Shanghai Jiao Tong University. High-quality single-shot transmission electron diffraction patterns have been recorded by scattering 2.5 MeV electrons off single crystalline gold and polycrystalline aluminum samples. The high quality diffraction pattern indicates an excellent spatial resolution, with the ratio of the diffraction ring radius over the ring rms width beyond 10. The electron pulse width is estimated to be about 300 fs. The high temporal and spatial resolution may open new opportunities inmore » various areas of sciences.« less

High quality single shot ultrafast MeV electron diffraction from a photocathode radio-frequency gun.

PubMed

Fu, Feichao; Liu, Shengguang; Zhu, Pengfei; Xiang, Dao; Zhang, Jie; Cao, Jianming

2014-08-01

A compact ultrafast electron diffractometer, consisting of an s-band 1.6 cell photocathode radio-frequency gun, a multi-function changeable sample chamber, and a sensitive relativistic electron detector, was built at Shanghai Jiao Tong University. High-quality single-shot transmission electron diffraction patterns have been recorded by scattering 2.5 MeV electrons off single crystalline gold and polycrystalline aluminum samples. The high quality diffraction pattern indicates an excellent spatial resolution, with the ratio of the diffraction ring radius over the ring rms width beyond 10. The electron pulse width is estimated to be about 300 fs. The high temporal and spatial resolution may open new opportunities in various areas of sciences.

Classification and assessment of retrieved electron density maps in coherent X-ray diffraction imaging using multivariate analysis.

PubMed

Sekiguchi, Yuki; Oroguchi, Tomotaka; Nakasako, Masayoshi

2016-01-01

Coherent X-ray diffraction imaging (CXDI) is one of the techniques used to visualize structures of non-crystalline particles of micrometer to submicrometer size from materials and biological science. In the structural analysis of CXDI, the electron density map of a sample particle can theoretically be reconstructed from a diffraction pattern by using phase-retrieval (PR) algorithms. However, in practice, the reconstruction is difficult because diffraction patterns are affected by Poisson noise and miss data in small-angle regions due to the beam stop and the saturation of detector pixels. In contrast to X-ray protein crystallography, in which the phases of diffracted waves are experimentally estimated, phase retrieval in CXDI relies entirely on the computational procedure driven by the PR algorithms. Thus, objective criteria and methods to assess the accuracy of retrieved electron density maps are necessary in addition to conventional parameters monitoring the convergence of PR calculations. Here, a data analysis scheme, named ASURA, is proposed which selects the most probable electron density maps from a set of maps retrieved from 1000 different random seeds for a diffraction pattern. Each electron density map composed of J pixels is expressed as a point in a J-dimensional space. Principal component analysis is applied to describe characteristics in the distribution of the maps in the J-dimensional space. When the distribution is characterized by a small number of principal components, the distribution is classified using the k-means clustering method. The classified maps are evaluated by several parameters to assess the quality of the maps. Using the proposed scheme, structure analysis of a diffraction pattern from a non-crystalline particle is conducted in two stages: estimation of the overall shape and determination of the fine structure inside the support shape. In each stage, the most accurate and probable density maps are objectively selected. The validity of the proposed scheme is examined by application to diffraction data that were obtained from an aggregate of metal particles and a biological specimen at the XFEL facility SACLA using custom-made diffraction apparatus.

Measuring Orbital Angular Momentum (OAM) States of Vortex Beams with Annular Gratings

PubMed Central

Zheng, Shuang; Wang, Jian

2017-01-01

Measuring orbital angular momentum (OAM) states of vortex beams is of great importance in diverse applications employing OAM-carrying vortex beams. We present a simple and efficient scheme to measure OAM states (i.e. topological charge values) of vortex beams with annular gratings. The magnitude of the topological charge value is determined by the number of dark fringes after diffraction, and the sign of the topological charge value is distinguished by the orientation of the diffraction pattern. We first theoretically study the diffraction patterns using both annular amplitude and phase gratings. The annular phase grating shows almost 10-dB better diffraction efficiency compared to the annular amplitude grating. We then experimentally demonstrate the OAM states measurement of vortex beams using annular phase grating. The scheme works well even for high-order vortex beams with topological charge value as high as ± 25. We also experimentally show the evolution of diffraction patterns when slightly changing the fractional topological charge value of vortex beam from 0.1 to 1.0. In addition, the proposed scheme shows potential large tolerance of beam alignment during the OAM states measurement of vortex beams. PMID:28094325

Continuous motion scan ptychography: Characterization for increased speed in coherent x-ray imaging

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

Deng, Junjing; Nashed, Youssef S. G.; Chen, Si

Ptychography is a coherent diffraction imaging (CDI) method for extended objects in which diffraction patterns are acquired sequentially from overlapping coherent illumination spots. The object’s complex transmission function can be reconstructed from those diffraction patterns at a spatial resolution limited only by the scattering strength of the object and the detector geometry. Most experiments to date have positioned the illumination spots on the sample using a move-settle-measure sequence in which the move and settle steps can take longer to complete than the measure step. We describe here the use of a continuous “fly-scan” mode for ptychographic data collection in whichmore » the sample is moved continuously, so that the experiment resembles one of integrating the diffraction patterns from multiple probe positions. This allows one to use multiple probe mode reconstruction methods to obtain an image of the object and also of the illumination function. We show in simulations, and in x-ray imaging experiments, some of the characteristics of fly-scan ptychography, including a factor of 25 reduction in the data acquisition time. This approach will become increasingly important as brighter x-ray sources are developed, such as diffraction limited storage rings.« less

Effect of the Chemical State of the Surface on the Relaxation of the Surface Shell Atoms in SiC and GaN Nanocrystals

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Weber, H. P.; Janik, J. F.; Palosz, W.; Curreri, Peter A. (Technical Monitor)

2002-01-01

The effect of the chemical state of the surface of nanoparticles on the relaxation in the near-surface layer was examined using the concept of the apparent lattice parameter (alp) determined for different diffraction vectors Q. The apparent lattice parameter is a lattice parameter determined either from an individual Bragg reflection, or from a selected region of the diffraction pattern. At low diffraction vectors the Bragg peak positions are affected mainly by the structure of the near-surface layer, while at high Q-values only the interior of the nano-grain contributes to the diffraction pattern. Following the measurements on raw (as prepared) powders we investigated powders cleaned by annealing at 400C under vacuum, and the same powders wetted with water. Theoretical alp-Q plots showed that the structure of the surface layer depends on the sample treatment. Semi-quantitative analysis based on the comparison of the experimental and theoretical alp-Q plots was performed. Theoretical alp-Q relations were obtained from the diffraction patterns calculated for models of nanocrystals with a strained surface layer using the Debye functions.

Measuring Orbital Angular Momentum (OAM) States of Vortex Beams with Annular Gratings.

PubMed

Zheng, Shuang; Wang, Jian

2017-01-17

Measuring orbital angular momentum (OAM) states of vortex beams is of great importance in diverse applications employing OAM-carrying vortex beams. We present a simple and efficient scheme to measure OAM states (i.e. topological charge values) of vortex beams with annular gratings. The magnitude of the topological charge value is determined by the number of dark fringes after diffraction, and the sign of the topological charge value is distinguished by the orientation of the diffraction pattern. We first theoretically study the diffraction patterns using both annular amplitude and phase gratings. The annular phase grating shows almost 10-dB better diffraction efficiency compared to the annular amplitude grating. We then experimentally demonstrate the OAM states measurement of vortex beams using annular phase grating. The scheme works well even for high-order vortex beams with topological charge value as high as ± 25. We also experimentally show the evolution of diffraction patterns when slightly changing the fractional topological charge value of vortex beam from 0.1 to 1.0. In addition, the proposed scheme shows potential large tolerance of beam alignment during the OAM states measurement of vortex beams.

Continuous motion scan ptychography: Characterization for increased speed in coherent x-ray imaging

DOE PAGES

Deng, Junjing; Nashed, Youssef S. G.; Chen, Si; ...

2015-02-23

Ptychography is a coherent diffraction imaging (CDI) method for extended objects in which diffraction patterns are acquired sequentially from overlapping coherent illumination spots. The object’s complex transmission function can be reconstructed from those diffraction patterns at a spatial resolution limited only by the scattering strength of the object and the detector geometry. Most experiments to date have positioned the illumination spots on the sample using a move-settle-measure sequence in which the move and settle steps can take longer to complete than the measure step. We describe here the use of a continuous “fly-scan” mode for ptychographic data collection in whichmore » the sample is moved continuously, so that the experiment resembles one of integrating the diffraction patterns from multiple probe positions. This allows one to use multiple probe mode reconstruction methods to obtain an image of the object and also of the illumination function. We show in simulations, and in x-ray imaging experiments, some of the characteristics of fly-scan ptychography, including a factor of 25 reduction in the data acquisition time. This approach will become increasingly important as brighter x-ray sources are developed, such as diffraction limited storage rings.« less

Continuous motion scan ptychography: characterization for increased speed in coherent x-ray imaging

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

Deng, Junjing; Nashed, Youssef S. G.; Chen, Si

2015-01-01

Ptychography is a coherent diffraction imaging (CDI) method for extended objects in which diffraction patterns are acquired sequentially from overlapping coherent illumination spots. The object's complex transmission function can be reconstructed from those diffraction patterns at a spatial resolution limited only by the scattering strength of the object and the detector geometry. Most experiments to date have positioned the illumination spots on the sample using a move-settle-measure sequence in which the move and settle steps can take longer to complete than the measure step. We describe here the use of a continuous "fly-scan" mode for ptychographic data collection in whichmore » the sample is moved continuously, so that the experiment resembles one of integrating the diffraction patterns from multiple probe positions. This allows one to use multiple probe mode reconstruction methods to obtain an image of the object and also of the illumination function. We show in simulations, and in x-ray imaging experiments, some of the characteristics of fly-scan ptychography, including a factor of 25 reduction in the data acquisition time. This approach will become increasingly important as brighter x-ray sources are developed, such as diffraction limited storage rings.« less

Continuous motion scan ptychography: characterization for increased speed in coherent x-ray imaging.

PubMed

Deng, Junjing; Nashed, Youssef S G; Chen, Si; Phillips, Nicholas W; Peterka, Tom; Ross, Rob; Vogt, Stefan; Jacobsen, Chris; Vine, David J

2015-03-09

Ptychography is a coherent diffraction imaging (CDI) method for extended objects in which diffraction patterns are acquired sequentially from overlapping coherent illumination spots. The object's complex transmission function can be reconstructed from those diffraction patterns at a spatial resolution limited only by the scattering strength of the object and the detector geometry. Most experiments to date have positioned the illumination spots on the sample using a move-settle-measure sequence in which the move and settle steps can take longer to complete than the measure step. We describe here the use of a continuous "fly-scan" mode for ptychographic data collection in which the sample is moved continuously, so that the experiment resembles one of integrating the diffraction patterns from multiple probe positions. This allows one to use multiple probe mode reconstruction methods to obtain an image of the object and also of the illumination function. We show in simulations, and in x-ray imaging experiments, some of the characteristics of fly-scan ptychography, including a factor of 25 reduction in the data acquisition time. This approach will become increasingly important as brighter x-ray sources are developed, such as diffraction limited storage rings.

In Situ 3D Coherent X-ray Diffraction Imaging of Shock Experiments: Possible?

NASA Astrophysics Data System (ADS)

Barber, John

2011-03-01

In traditional coherent X-ray diffraction imaging (CXDI), a 2D or quasi-2D object is illuminated by a beam of coherent X-rays to produce a diffraction pattern, which is then manipulated via a process known as iterative phase retrieval to reconstruct an image of the original 2D sample. Recently, there have been dramatic advances in methods for performing fully 3D CXDI of a sample from a single diffraction pattern [Raines et al, Nature 463 214-7 (2010)], and these methods have been used to image samples tens of microns in size using soft X-rays. In this work, I explore the theoretical possibility of applying 3D CXDI techniques to the in situ imaging of the interaction between a shock front and a polycrystal, a far more stringent problem. A delicate trade-off is required between photon energy, spot size, imaging resolution, and the dimensions of the experimental setup. In this talk, I will outline the experimental and computational requirements for performing such an experiment, and I will present images and movies from simulations of one such hypothetical experiment, including both the time-resolved X-ray diffraction patterns and the time-resolved sample imagery.

Effect of fluorine doping on highly transparent conductive spray deposited nanocrystalline tin oxide thin films

NASA Astrophysics Data System (ADS)

Moholkar, A. V.; Pawar, S. M.; Rajpure, K. Y.; Bhosale, C. H.; Kim, J. H.

2009-09-01

The undoped and fluorine doped thin films are synthesized by using cost-effective spray pyrolysis technique. The dependence of optical, structural and electrical properties of SnO 2 films, on the concentration of fluorine is reported. Optical absorption, X-ray diffraction, scanning electron microscope (SEM) and Hall effect studies have been performed on SnO 2:F (FTO) films coated on glass substrates. The film thickness varies from 800 to 1572 nm. X-ray diffraction pattern reveals the presence of cassiterite structure with (2 0 0) preferential orientation for FTO films. The crystallite size varies from 35 to 66 nm. SEM and AFM study reveals the surface of FTO to be made of nanocrystalline particles. The electrical study reveals that the films are degenerate and exhibit n-type electrical conductivity. The 20 wt% F doped film has a minimum resistivity of 3.8 × 10 -4 Ω cm, carrier density of 24.9 × 10 20 cm -3 and mobility of 6.59 cm 2 V -1 s -1. The sprayed FTO film having minimum resistance of 3.42 Ω/cm 2, highest figure of merit of 6.18 × 10 -2 Ω -1 at 550 nm and 96% IR reflectivity suggest, these films are useful as conducting layers in electrochromic and photovoltaic devices and also as the passive counter electrode.

Note on use of slope diffraction coefficients for aperture antennas on finite ground planes

NASA Technical Reports Server (NTRS)

Cockrell, C. R.; Beck, F. B.

1995-01-01

The use of slope diffraction coefficients along with regular diffraction coefficients for calculating the radiation patterns of aperture antennas in a finite ground plane is investigated. Explicit expressions for regular diffraction coefficients and slope diffraction coefficients are presented. The expressions for the incident magnetic field in terms of the magnetic current in the aperture are given. The slope of the incident magnetic field is calculated and closed form expressions are presented.

Segal crystallinity index revisited by the simulation of x-ray diffraction patterns of cotton cellulose IB and cellulose II

USDA-ARS?s Scientific Manuscript database

The Segal method estimates the amorphous fraction of cellulose IB materials simply based on intensity at 18o 20 in an X-ray diffraction pattern and was extended to cellulose II using 16o 2O intensity. To address the dependency of Segal amorphous intensity on crystal size, cellulose polymorph, and th...

Diffraction gratings used as identifying markers

DOEpatents

Deason, V.A.; Ward, M.B.

1991-03-26

A finely detailed diffraction grating is applied to an object as an identifier or tag which is unambiguous, difficult to duplicate, or remove and transfer to another item, and can be read and compared with prior readings with relative ease. The exact pattern of the diffraction grating is mapped by diffraction moire techniques and recorded for comparison with future readings of the same grating. 7 figures.

Diffraction of a Gaussian Beam by a Spherical Obstacle

NASA Technical Reports Server (NTRS)

Lock, James A.; Hovenac, Edward A.

1993-01-01

The Kirchhoff integral for diffraction in the near-forward direction is derived from the exact solution of the electromagnetic boundary value problem of a focused Gaussian laser beam incident on a spherical particle. The diffracted intensity in the vicinity of the particle is computed and the way in which the features of the diffraction pattern depend on the width of the Gaussian beam is commented on.

Molecular organization of the cholesteryl ester droplets in the fatty streaks of human aorta.

PubMed Central

Engelman, D M; Hillman, G M

1976-01-01

X-ray diffraction patterns from human arterial specimens containing atherosclerotic fatty streak lesions exhibited a single sharp reflection, corresponding to a structural spacing of about 35 A. Specimens without lesions did not. When specimens with fatty streaks were heated, an order-to-disorder phase transition was revealed by the disappearance of the sharp reflection. The transition was thermally reversible and its temperature varied from aorta to aorta over a range from 28 degrees to 42 degrees C. Since cholesteryl ester droplets are a major component of fatty streaks, comparison studies were made of the diffraction behavior from pure cholesteryl esters. We found that the diffraction patterns of the fatty streak material could be accounted for by the organization of the cholesteryl esters into a liquid-crystalline smectic phase that melts from the smectic to a less ordered phase upon heating. When combined with the conclusions of others from polarized light microscopy, our study shows that a droplet in the smectic phase has well-defined concentric layers of lipid molecules. In each layer, the long axes of the molecules have a net radial orientation with respect to the droplet, but the side-to-side organization is disordered. We suggest that the accessibility of portions of the lipids for specific binding to enzymes or transport proteins may be restricted when they are in the smectic state, and that exchange of lipids with surrounding membranes or other potential binding sites may likewise be inhibited. The restriction in the smectic phase should be greater than in the less ordered phases that exist at higher temperatures. Images PMID:965500

Mulberry leaf extract mediated synthesis of gold nanoparticles and its anti-bacterial activity against human pathogens

NASA Astrophysics Data System (ADS)

Adavallan, K.; Krishnakumar, N.

2014-06-01

Gold nanoparticles (Au-NPs) were synthesized at room temperature using Morus alba (mulberry) leaf extract as reducing and stabilizing agent. The development of plant mediated synthesis of nanoparticles is gaining importance due to its simplicity, low cost, non-toxicity, eco-friendliness, long term stability and reproducible aqueous synthesis method to obtain a self-assembly of nearly monodispersed Au-NPs. The formation and morphology of biosynthesized nanoparticles are investigated with the help of UV-Vis spectroscopy, dynamic light scattering (DLS), transmission electron microscopy (TEM), atomic force microscopy (AFM), x-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR) techniques. Au-NPs formation was screened by UV-Vis spectroscopy through color conversion due to surface plasmon resonance band at 538 nm for Au-NPs. DLS studies revealed that the average size of Au-NPs was 50 nm. TEM studies showed the particles to be nearly spherical with few irregular shapes and particle size ranges 15-53 nm. The AFM image clearly shows the surface morphology of the well-dispersed Au-NPs with less than 50 nm. The high crystallinity of nanoparticles is evident from bright circular spots in the selected area electron diffraction (SAED) pattern. X-ray diffraction pattern showed high purity and face-centered cubic structure of Au-NPs. The FT-IR results indicate the presence of different functional groups present in the biomolecule capping the nanoparticles. Further, biosynthesized Au-NPs show strong zone of inhibition against Vibrio cholera (gram-negative) and Staphylococcus aureus (gram-positive) whereas, chemically synthesized Au-NPs and mulberry leaf extract exhibit a fair zone of inhibition.

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.

Amorphous Analogs of Martian Global Soil: Pair Distribution Function Analyses and Implications for Scattering Models of Chemin X-ray Diffraction Data

NASA Technical Reports Server (NTRS)

Achilles, C. N.; Bish, D. L.; Rampe, E. B.; Morris, R. V.

2015-01-01

Soils on Mars have been analyzed by the Mars Exploration Rovers (MER) and most recently by the Mars Science Laboratory (MSL) rover. Chemical analyses from a majority of soil samples suggest that there is a relatively uniform global soil composition across much of the planet. A soil site, Rocknest, was sampled by the MSL science payload including the CheMin X-ray diffractometer and the Alpha Particle X-ray Spectrometer (APXS). Che- Min X-ray diffraction (XRD) data revealed crystalline phases and a broad, elevated background, indicating the presence of amorphous or poorly ordered materials (Fig 1). Based on the chemical composition of the bulk soil measured by APXS and the composition of crystalline phases derived from unit-cell parameters determined with CheMin data, the percentages of crystalline and amorphous phases were calculated at 51% and 49%, respectively. Attempts to model the amorphous contribution to CheMin XRD patterns were made using amorphous standards and full-pattern fitting methods and show that the broad, elevated background region can be fitted by basaltic glass, allophane, and palagonite. However, the modeling shows only that these phases have scattering patterns similar to that for the soil, not that they represent unique solutions. Here, we use pair distribution function (PDF) analysis to determine the short-range order of amorphous analogs in martian soils and better constrain the amorphous material detected by CheMin.

Three-Dimensional Reconstruction of the Giant Mimivirus Particle with an X-Ray Free-Electron Laser (CXIDB ID 30)

DOE Data Explorer

Ekeberg, Tomas

2015-05-26

This dataset contains the diffraction patterns that were used for the first three-dimensional reconstruction of a virus using FEL data. The sample was the giant mimivirus particle, which is one of the largest known viruses with a diameter of 450 nm. The dataset consists of the 198 diffraction patterns that were used in the analysis.

Devices useful for vacuum ultraviolet beam characterization including a movable stage with a transmission grating and image detector

DOEpatents

Gessner, Oliver; Kornilov, Oleg A; Wilcox, Russell B

2013-10-29

The invention provides for a device comprising an apparatus comprising (a) a transmission grating capable of diffracting a photon beam into a diffracted photon output, and (b) an image detector capable of detecting the diffracted photon output. The device is useful for measuring the spatial profile and diffraction pattern of a photon beam, such as a vacuum ultraviolet (VUV) beam.

Theory and Application of Auger and Photoelectron Diffraction and Holography

NASA Astrophysics Data System (ADS)

Chen, Xiang

This dissertation addresses the theories and applications of three important surface analysis techniques: Auger electron diffraction (AED), x-ray photoelectron diffraction (XPD), and Auger and photoelectron holography. A full multiple-scattering scheme for the calculations of XPD, AED, and Kikuchi electron diffraction pattern from a surface cluster is described. It is used to simulate 64 eV M_{2,3}VV and 913 eV L_3VV AED patterns from Cu(001) surfaces, in order to test assertions in the literature that they are explicable by a classical "blocking" and channeling model. We find that this contention is not valid, and that only a quantum mechanical multiple-scattering calculation is able to simulate these patterns well. The same multiple scattering simulation scheme is also used to investigate the anomalous phenomena of peak shifts off the forward-scattering directions in photo -electron diffraction patterns of Mg KLL (1180 eV) and O 1s (955 eV) from MgO(001) surfaces. These shifts are explained by calculations assuming a short electron mean free path. Similar simulations of XPD from a CoSi_2(111) surface for Co-3p and Si-2p normal emission agree well with experimental diffraction patterns. A filtering process aimed at eliminating the self -interference effect in photoelectron holography is developed. A better reconstructed image from Si-2p XPD from a Si(001) (2 times 1) surface is seen at atomic resolution. A reconstruction algorithm which corrects for the anisotropic emitter waves as well as the anisotropic atomic scattering factors is used for holographic reconstruction from a Co-3p XPD pattern from a CoSi_2 surface. This new algorithm considerably improves the reconstructed image. Finally, a new reconstruction algorithm called "atomic position recovery by iterative optimization of reconstructed intensities" (APRIORI), which takes account of the self-interference terms omitted by the other holographic algorithms, is developed. Tests on a Ni-C-O chain and Si(111)(sqrt{3} times sqrt{3})B surface suggest that this new method may overcome the twin image problem in the traditional holographic methods, reduce the artifacts in real space, and even separately identify the chemical species of the scatterers.

Absolute angular encoder based on optical diffraction

NASA Astrophysics Data System (ADS)

Wu, Jian; Zhou, Tingting; Yuan, Bo; Wang, Liqiang

2015-08-01

A new encoding method for absolute angular encoder based on optical diffraction was proposed in the present study. In this method, an encoder disc is specially designed that a series of elements are uniformly spaced in one circle and each element is consisted of four diffraction gratings, which are tilted in the directions of 30°, 60°, -60° and -30°, respectively. The disc is illuminated by a coherent light and the diffractive signals are received. The positions of diffractive spots are used for absolute encoding and their intensities are for subdivision, which is different from the traditional optical encoder based on transparent/opaque binary principle. Since the track's width in the disc is not limited in the diffraction pattern, it provides a new way to solve the contradiction between the size and resolution, which is good for minimization of encoder. According to the proposed principle, the diffraction pattern disc with a diameter of 40 mm was made by lithography in the glass substrate. A prototype of absolute angular encoder with a resolution of 20" was built up. Its maximum error was tested as 78" by comparing with a small angle measuring system based on laser beam deflection.

Specimen preparation for cryogenic coherent X-ray diffraction imaging of biological cells and cellular organelles by using the X-ray free-electron laser at SACLA

PubMed Central

Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka; Okajima, Koji; Fukuda, Asahi; Oide, Mao; Yamamoto, Masaki; Nakasako, Masayoshi

2016-01-01

Coherent X-ray diffraction imaging (CXDI) allows internal structures of biological cells and cellular organelles to be analyzed. CXDI experiments have been conducted at 66 K for frozen-hydrated biological specimens at the SPring-8 Angstrom Compact Free-Electron Laser facility (SACLA). In these cryogenic CXDI experiments using X-ray free-electron laser (XFEL) pulses, specimen particles dispersed on thin membranes of specimen disks are transferred into the vacuum chamber of a diffraction apparatus. Because focused single XFEL pulses destroy specimen particles at the atomic level, diffraction patterns are collected through raster scanning the specimen disks to provide fresh specimen particles in the irradiation area. The efficiency of diffraction data collection in cryogenic experiments depends on the quality of the prepared specimens. Here, detailed procedures for preparing frozen-hydrated biological specimens, particularly thin membranes and devices developed in our laboratory, are reported. In addition, the quality of the frozen-hydrated specimens are evaluated by analyzing the characteristics of the collected diffraction patterns. Based on the experimental results, the internal structures of the frozen-hydrated specimens and the future development for efficient diffraction data collection are discussed. PMID:27359147

Specimen preparation for cryogenic coherent X-ray diffraction imaging of biological cells and cellular organelles by using the X-ray free-electron laser at SACLA.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka; Okajima, Koji; Fukuda, Asahi; Oide, Mao; Yamamoto, Masaki; Nakasako, Masayoshi

2016-07-01

Coherent X-ray diffraction imaging (CXDI) allows internal structures of biological cells and cellular organelles to be analyzed. CXDI experiments have been conducted at 66 K for frozen-hydrated biological specimens at the SPring-8 Angstrom Compact Free-Electron Laser facility (SACLA). In these cryogenic CXDI experiments using X-ray free-electron laser (XFEL) pulses, specimen particles dispersed on thin membranes of specimen disks are transferred into the vacuum chamber of a diffraction apparatus. Because focused single XFEL pulses destroy specimen particles at the atomic level, diffraction patterns are collected through raster scanning the specimen disks to provide fresh specimen particles in the irradiation area. The efficiency of diffraction data collection in cryogenic experiments depends on the quality of the prepared specimens. Here, detailed procedures for preparing frozen-hydrated biological specimens, particularly thin membranes and devices developed in our laboratory, are reported. In addition, the quality of the frozen-hydrated specimens are evaluated by analyzing the characteristics of the collected diffraction patterns. Based on the experimental results, the internal structures of the frozen-hydrated specimens and the future development for efficient diffraction data collection are discussed.

Computational modeling and experimental characterization of bacterial microcolonies for rapid detection using light scattering

NASA Astrophysics Data System (ADS)

Bai, Nan

A label-free and nondestructive optical elastic forward light scattering method has been extended for the analysis of microcolonies for food-borne bacteria detection and identification. To understand the forward light scattering phenomenon, a model based on the scalar diffraction theory has been employed: a bacterial colony is considered as a biological spatial light modulator with amplitude and phase modulation to the incoming light, which continues to propagate to the far-field to form a distinct scattering 'fingerprint'. Numerical implementation via angular spectrum method (ASM) and Fresnel approximation have been carried out through Fast Fourier Transform (FFT) to simulate this optical model. Sampling criteria to achieve unbiased and un-aliased simulation results have been derived and the effects of violating these conditions have been studied. Diffraction patterns predicted by these two methods (ASM and Fresnel) have been compared to show their applicability to different simulation settings. Through the simulation work, the correlation between the colony morphology and its forward scattering pattern has been established to link the number of diffraction rings and the half cone angle with the diameter and the central height of the Gaussian-shaped colonies. In order to experimentally prove the correlation, a colony morphology analyzer has been built and used to characterize the morphology of different bacteria genera and investigate their growth dynamics. The experimental measurements have demonstrated the possibility of differentiating bacteria Salmonella, Listeria, Escherichia in their early growth stage (100˜500 µm) based on their phenotypic characteristics. This conclusion has important implications in microcolony detection, as most bacteria of our interest need much less incubation time (8˜12 hours) to grow into this size range. The original forward light scatterometer has been updated to capture scattering patterns from microcolonies. Experiments have been performed to reveal the time dependent nature of scattering patterns. The experimental work has been compared with simulation results and demonstrated the feasibility of extending this technique for microcolony identification. Lastly, a quantitative phase imaging technique based on the phase gradient driven intensity variation has been studied and implemented to render the 2D phase map of the colony sample.

Grazing incidence x-ray diffraction analysis of zeolite NaA membranes on porous alumina tubes.

PubMed

Kyotani, Tomohiro

2006-07-01

Zeolite NaA-type membranes hydrothermally synthesized on porous alumina tubes, for dehydration process, were characterized by grazing incidence 2 theta scan X-ray diffraction analysis (GIXRD). The fine structure of the membrane was studied fractionally for surface layer and for materials embedded in the porous alumina tube. The thickness of the surface layer on the porous alumina tube in the membranes used in this study was approximately 2-3 microm as determined from transmission electron microscopy with focused ion beam thin-layer specimen preparation technique (FIB-TEM). To discuss the effects of the membrane surface morphology on the GIXRD measurements, CaA-type membrane prepared by ion exchange from the NaA-type membrane and surface-damaged NaA-type membrane prepared by water leaching were also studied. For the original NaA-type membrane, 2 theta scan GIXRD patterns could be clearly measured at X-ray incidence angles (alpha) ranging from 0.1 to 2.0 deg in increments of 0.1 deg. The surface layers of the 2 - 3 microm on the porous alumina tube correspond to the alpha values up to ca. 0.2 deg. For the CaA-type and the surface-damaged NaA-type membranes, however, diffraction patterns from the surface layer could not be successfully detected and the others were somewhat broad. For all the three samples, diffraction intensities of both zeolite and alumina increased with depth (X-ray incidence angle, alpha) in the porous alumina tube region. The depth profile analysis of the membranes based on the GIXRD first revealed that amount of zeolite crystal embedded in the porous alumina tube is much larger than that in the surface layer. Thus, the 2 theta scan GIXRD is a useful method to study zeolite crystal growth mechanism around (both inside and outside) the porous alumina support during hydrothermal synthesis and to study water permeation behavior in the dehydration process.

Stacking fault induced tunnel barrier in platelet graphite nanofiber

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

Lan, Yann-Wen, E-mail: chiidong@phys.sinica.edu.tw, E-mail: ywlan@phys.sinica.edu.tw; Chang, Yuan-Chih; Chang, Chia-Seng

A correlation study using image inspection and electrical characterization of platelet graphite nanofiber devices is conducted. Close transmission electron microscopy and diffraction pattern inspection reveal layers with inflection angles appearing in otherwise perfectly stacked graphene platelets, separating nanofibers into two domains. Electrical measurement gives a stability diagram consisting of alternating small-large Coulomb blockade diamonds, suggesting that there are two charging islands coupled together through a tunnel junction. Based on these two findings, we propose that a stacking fault can behave as a tunnel barrier for conducting electrons and is responsible for the observed double-island single electron transistor characteristics.

Synthesis on structure and properties of zinc nanocrystal in high ordered 3D nanostructures

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

Sathyaseelan, B., E-mail: bsseelan03@gmail.com; Manigandan, A.; Anbarasu, V.

2015-06-24

The wet impregnation method was employed to prepare ZnO encapsulated in mesoporous silica (ZnO/KIT-6). The prepared ZnO/KIT-6 samples have been studied by X-ray diffraction, transmission electron microscope, and nitrogen adsorption–desorption isotherm. The low angle powder XRD patterns of Calcined ZnO/KIT-6 materials showed a phase that can be indexed to cubic Ia3d. Tem images revealed well ordered cubic 3D nanoporous chennels. The ZnO encapsulated in KIT-6 can be used as light-emitting diodes and ultraviolet nanolasers.

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

Park, J.; Ahn, Y.; Tilka, J. A.

Disorder in the potential-energy landscape presents a major obstacle to the more rapid development of semiconductor quantum device technologies. We report a large-magnitude source of disorder, beyond commonly considered unintentional background doping or fixed charge in oxide layers: nanoscale strain fields induced by residual stresses in nanopatterned metal gates. Quantitative analysis of synchrotron coherent hard x-ray nanobeam diffraction patterns reveals gate-induced curvature and strains up to 0.03% in a buried Si quantum well within a Si/SiGe heterostructure. Furthermore, electrode stress presents both challenges to the design of devices and opportunities associated with the lateral manipulation of electronic energy levels.

3-dimensional indexation of the icosahedral diffraction pattern using the techniques of electron microscopy

NASA Astrophysics Data System (ADS)

Bourdillon, Antony

2012-11-01

The following facts about icosahedra need wider attention. 1) The golden section τ is as fundamental to the icosahedral structure (length /edge) as π is to the sphere (circumference /diameter). 2) The diffraction series are in restricted Fibonacci order because the ratio of adjacent terms fn/fn-1 does not vary, but is the constant τ. The series is therefore geometric. 3) Because of the tetragonal subgroup in the icosahedral point group symmetry, many axes in the icosahedral structure have identical orientation to axes in the face centered cubic matrix of Al6Mn [1] (e.g. [100] and [111]). On these bases, a three dimensional stereographic projection will be presented. 4) A quasi-Bragg law is derived that correctly represents the diffraction series in powers of τ [2]. Furthermore, by employing the normal conventions of electron microscopy, all diffraction patterns are completely indexed in three dimensions. These are the topic of this presentation. Significant consequences will be presented elsewhere: 1) The diffraction pattern intensities near all main axes are correctly simulated, and all atoms are located on a specimen image. 2) The quasi-Bragg law has a special metric. Atomic locations are consistently calculated for the first time. 3) Whereas the Bragg law transforms a crystal lattice in real space into a reciprocal lattice in diffraction space, the quasi-Bragg law transforms a geometric diffraction pattern into a hierarchic structure. 4) Hyperspatial indexation [3] is superceded. [1] Shechtman, D.; Blech, I.; Gratias, D.; Cahn, J.W., Metallic phase with long-range orientational order and no translational symmetry, Phys. Rev. Lett., 1984, 53, 1951-3. [2] Bourdillon, A. J., Nearly free electron band structures in a logarithmically periodic solid, Sol. State Comm. 2009, 149, 1221-1225. [3] Duneau, M., and Katz, A., Phys Rev Lett 54, 2688-2691

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.

Structural, vibrational and dielectric studies of (0.95)Pb(Zr{sub x}Ti{sub 1−x})O{sub 3}-(0.05)BiFeO{sub 3} nanoceramics

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

Sharma, Subhash, E-mail: rk.dwivedi@jiit.ac.in; Singh, Vikash, E-mail: rk.dwivedi@jiit.ac.in; Dwivedi, R. K., E-mail: rk.dwivedi@jiit.ac.in

2014-04-24

(0.95)Pb(Zr{sub x}Ti{sub 1−x})O{sub 3}-(0.05)BiFeO{sub 3} nanoceramics with x=0.51, 0.53 and 0.55 were synthesized by sol-gel route. Rietveld refined X-ray powder diffraction pattern of the samples confirm the single phase formation of compounds with tetragonal structure (P4mm). FT-IR studies revealed that slight shift of phonon modes towards the lower wave number and increase in the bond length with increasing Zr{sup 4+} concentration. Room temperature dielectric properties of system revealed that relaxor characteristics of these samples. Ferroelectric hysteresis curve shows the decrease in polarization values with Zr concentration.

Detection of magnetic circular dichroism in amorphous materials utilizing a single-crystalline overlayer

DOE PAGES

Lin, J.; Zhong, X. Y.; Song, C.; ...

2017-12-27

Physicists are fascinated with topological defects in solid-state materials, because by breaking the translational symmetry they offer emerging properties that are not present in their parental phases. For example, edge dislocations—the 2π phase-winding topological defects—in antiferromagnetic NiO crystals can exhibit ferromagnetic behaviors. Herein, we study how these defects could give rise to exotic topological orders when they interact with a high energy electron beam. To probe this interaction, we formed a coherent electron nanobeam in a scanning transmission electron microscope and recorded the far-field transmitted patterns as the beam steps through the edge dislocation core in [001] NiO. Surprisingly, wemore » found the amplitude patterns of the <020> Bragg disks evolve in a similar manner to the evolution of an annular solar eclipse. Using the ptychographic technique, we recovered the missing phase information in the diffraction plane and revealed the topological phase vortices in the diffracted beams. Through atomic topological defects, the wave function of electrons can be converted from plane wave to electron vortex. This approach provides a new perspective for boosting the collection efficiency of magnetic circular dichroism spectra with high spatial resolution and understanding the relationship between symmetry breaking and exotic property of individual topological defect at atomic level.« less

Detection of magnetic circular dichroism in amorphous materials utilizing a single-crystalline overlayer

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

Lin, J.; Zhong, X. Y.; Song, C.

Physicists are fascinated with topological defects in solid-state materials, because by breaking the translational symmetry they offer emerging properties that are not present in their parental phases. For example, edge dislocations—the 2π phase-winding topological defects—in antiferromagnetic NiO crystals can exhibit ferromagnetic behaviors. Herein, we study how these defects could give rise to exotic topological orders when they interact with a high energy electron beam. To probe this interaction, we formed a coherent electron nanobeam in a scanning transmission electron microscope and recorded the far-field transmitted patterns as the beam steps through the edge dislocation core in [001] NiO. Surprisingly, wemore » found the amplitude patterns of the <020> Bragg disks evolve in a similar manner to the evolution of an annular solar eclipse. Using the ptychographic technique, we recovered the missing phase information in the diffraction plane and revealed the topological phase vortices in the diffracted beams. Through atomic topological defects, the wave function of electrons can be converted from plane wave to electron vortex. This approach provides a new perspective for boosting the collection efficiency of magnetic circular dichroism spectra with high spatial resolution and understanding the relationship between symmetry breaking and exotic property of individual topological defect at atomic level.« less

Diffraction enhanced kinetic depth X-ray imaging

NASA Astrophysics Data System (ADS)

Dicken, A.

An increasing number of fields would benefit from a single analytical probe that can characterise bulk objects that vary in morphology and/or material composition. These fields include security screening, medicine and material science. In this study the X-ray region is shown to be an effective probe for the characterisation of materials. The most prominent analytical techniques that utilise X-radiation are reviewed. The study then focuses on methods of amalgamating the three dimensional power of kinetic depth X-ray (KDFX) imaging with the materials discrimination of angular dispersive X-ray diffraction (ADXRD), thus providing KDEX with a much needed material specific counterpart. A knowledge of the sample position is essential for the correct interpretation of diffraction signatures. Two different sensor geometries (i.e. circumferential and linear) that are able to collect end interpret multiple unknown material diffraction patterns and attribute them to their respective loci within an inspection volume are investigated. The circumferential and linear detector geometries are hypothesised, simulated and then tested in an experimental setting with the later demonstrating a greater ability at discerning between mixed diffraction patterns produced by differing materials. Factors known to confound the linear diffraction method such as sample thickness and radiation energy have been explored and quantified with a possible means of mitigation being identified (i.e. via increasing the sample to detector distance). A series of diffraction patterns (following the linear diffraction approach) were obtained from a single phantom object that was simultaneously interrogated via KDEX imaging. Areas containing diffraction signatures matched from a threat library have been highlighted in the KDEX imagery via colour encoding and match index is inferred by intensity. This union is the first example of its kind and is called diffraction enhanced KDEX imagery. Finally an additional source of information obtained from object disparity is explored as an alternative means of calculating sample loci. This offers a greater level of integration between these two complimentary techniques as object disparity could be used to reinforce the results produced by the linear diffraction geometry.

Optofluidic two-dimensional grating volume refractive index sensor.

PubMed

Sarkar, Anirban; Shivakiran Bhaktha, B N; Khastgir, Sugata Pratik

2016-09-10

We present an optofluidic reservoir with a two-dimensional grating for a lab-on-a-chip volume refractive index sensor. The observed diffraction pattern from the device resembles the analytically obtained fringe pattern. The change in the diffraction pattern has been monitored in the far-field for fluids with different refractive indices. Reliable measurements of refractive index variations, with an accuracy of 6×10^-3 refractive index units, for different fluids establishes the optofluidic device as a potential on-chip tool for monitoring dynamic refractive index changes.

Comment on Sub-15 nm Hard X-Ray Focusing with a New Total-Reflection Zone Plate

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

Specht, Eliot D

2011-01-01

Takano et al. report the focusing of 10-keV X-rays to a size of 14.4 nm using a total-reflection zone plate (TRZP). This focal size is at the diffraction limit for the optic's aperture. This would be a noteworthy result, since the TRZP was fabricated using conventional lithography techniques. Alternative nanofocusing optics require more demanding fabrication methods. However, as I will discuss in this Comment, the intensity distribution presented by Takano et al. (Fig. 4 of ref. 1) is more consistent with the random speckle pattern produced by the scattering of a coherent incident beam by a distorted optic than withmore » a diffraction-limited focus. When interpreted in this manner, the true focal spot size is {approx}70 nm: 5 times the diffraction limit. When a coherent photon beam illuminates an optic containing randomly distributed regions which introduce different phase shifts, the scattered diffraction pattern consists of a speckle pattern. Each speckle will be diffraction-limited: the peak width of a single speckle depends entirely on the source coherence and gives no information about the optic. The envelope of the speckle distribution corresponds to the focal spot which would be observed using incoherent illumination. The width of this envelope is due to the finite size of the coherently-diffracting domains produced by slope and position errors in the optic. The focal intensity distribution in Fig. 4 of ref. 1 indeed contains a diffraction-limited peak, but this peak contains only a fraction of the power in the focused, and forms part of a distribution of sharp peaks with an envelope {approx}70 nm in width, just as expected for a speckle pattern. At the 4mm focal distance, the 70 nm width corresponds to a slope error of 18 {micro}rad. To reach the 14 nm diffraction limit, the slope error must be reduced to 3 {micro}rad. Takano et al. have identified a likely source of this error: warping due to stress as a result of zone deposition. It will be interesting to see whether the use of a more rigid substrate gives improved results.« less

Random technique to encode complex valued holograms with on axis reconstruction onto phase-only displays.

PubMed

Luis Martínez Fuentes, Jose; Moreno, Ignacio

2018-03-05

A new technique for encoding the amplitude and phase of diffracted fields in digital holography is proposed. It is based on a random spatial multiplexing of two phase-only diffractive patterns. The first one is the phase information of the intended pattern, while the second one is a diverging optical element whose purpose is the control of the amplitude. A random number determines the choice between these two diffractive patterns at each pixel, and the amplitude information of the desired field governs its discrimination threshold. This proposed technique is computationally fast and does not require iterative methods, and the complex field reconstruction appears on axis. We experimentally demonstrate this new encoding technique with holograms implemented onto a flicker-free phase-only spatial light modulator (SLM), which allows the axial generation of such holograms. The experimental verification includes the phase measurement of generated patterns with a phase-shifting polarization interferometer implemented in the same experimental setup.

High-speed autofocusing of a cell using diffraction pattern

NASA Astrophysics Data System (ADS)

Oku, Hiromasa; Ishikawa, Masatoshi; Theodorus; Hashimoto, Koichi

2006-05-01

This paper proposes a new autofocusing method for observing cells under a transmission illumination. The focusing method uses a quick and simple focus estimation technique termed “depth from diffraction,” which is based on a diffraction pattern in a defocused image of a biological specimen. Since this method can estimate the focal position of the specimen from only a single defocused image, it can easily realize high-speed autofocusing. To demonstrate the method, it was applied to continuous focus tracking of a swimming paramecium, in combination with two-dimensional position tracking. Three-dimensional tracking of the paramecium for 70 s was successfully demonstrated.

Resolution of 90 nm (lambda/5) in an optical transmission microscope with an annular condenser.

PubMed

Vainrub, Arnold; Pustovyy, Oleg; Vodyanoy, Vitaly

2006-10-01

Resolution of 90 nm was achieved with a research microscope simply by replacing the standard bright-field condenser with a homebuilt illumination system with a cardioid annular condenser. Diffraction gratings with 100 nm width lines as well as less than 100 nm size features of different-shaped objects were clearly visible on a calibrated microscope test slide. The resolution increase results from a known narrower diffraction pattern in coherent illumination for the annular aperture compared with the circular aperture. This explanation is supported by an excellent accord of calculated and measured diffraction patterns for a 50 nm radius disk.

Local nanoscale strain mapping of a metallic glass during in situ testing

NASA Astrophysics Data System (ADS)

Gammer, Christoph; Ophus, Colin; Pekin, Thomas C.; Eckert, Jürgen; Minor, Andrew M.

2018-04-01

The local elastic strains during tensile deformation in a CuZrAlAg metallic glass are obtained by fitting an elliptic shape function to the characteristic amorphous ring in electron diffraction patterns. Scanning nanobeam electron diffraction enables strain mapping with a resolution of a few nanometers. Here, a fast direct electron detector is used to acquire the diffraction patterns at a sufficient speed to map the local transient strain during continuous tensile loading in situ in the transmission electron microscope. The elastic strain in tensile direction was found to increase during loading. After catastrophic fracture, a residual elastic strain that relaxes over time was observed.

UHV-TEM/TED observation of Ag islands grown on Si( 1 1 1 ) 3× 3-Ag surface

NASA Astrophysics Data System (ADS)

Oshima, Yoshifumi; Nakade, Hiroyuki; Shigeki, Sinya; Hirayama, Hiroyuki; Takayanagi, Kunio

2001-11-01

Growths of Ag islands on Si(1 1 1)3×3-Ag surface at room temperature were observed by UHV transmission electron microscopy and diffraction. The Ag islands grown after six monolayer deposition had neither (1 0 0) nor (1 1 0) orientation, but had two complex epitaxial orientations dominantly. One was striped islands which gave rise to a diffraction pattern commensurate with the 3×3 lattice of the Si(1 1 1) surface. The other was the coagulated islands whose diffraction pattern indicated the Ag(1 -3 4) sheet grown parallel to the Si(1 1 1) surface.

Diffractive optics for particle velocimetry and sizing

NASA Technical Reports Server (NTRS)

Wilson, D. W.; Gogna, P. K.; Chacon, R. J.; Muller, R. E.; Fourguette, D.; Modarress, D.; Taugwalder, F.; Svitek, P.; Gharib, M.

2002-01-01

Beam-shaping diffractive optical elements are used to create structured light patterns in fluid flows. Particle scattering results in detected signals that can be used to determine the particle size and velocity.

Effect of Service Stress on Impact Resistance, X-ray Diffraction Patterns, and Microstructure of 25s Aluminum Alloy

NASA Technical Reports Server (NTRS)

Kies, J A; Quick, G W

1939-01-01

Report presents the results of a great number of tests made to determine the effect of service stresses on the impact resistance, the x-ray diffraction patterns, and the microstructure of 25s aluminum alloy. Many of the specimens were taken from actual propeller blades and others were cut from 13/16-inch rod furnished by the Aluminum Company of America.

Collimation testing using slit Fresnel diffraction

NASA Astrophysics Data System (ADS)

Luo, Xiaohe; Hui, Mei; Wang, Shanshan; Hou, Yinlong; Zhou, Siyu; Zhu, Qiudong

2018-03-01

A simple collimation testing method based on slit Fresnel diffraction is proposed. The method needs only a CMOS and a slit with no requirement in dimensional accuracy. The light beam to be tested diffracts across the slit and forms a Fresnel diffraction pattern received by CMOS. After analysis, the defocusing amount and the distance between the primary peak point and secondary peak point of diffraction pattern fulfill an expression relationship and then the defocusing amount can be deduced from the expression. The method is applied to both the coherent beam and partially coherent beam, and these two beams are emitted from a laser and light-emitting diode (LED) with a spectrum width of about 50 nm in this paper. Simulations show that the wide spectrum of LED has the effect of smooth filtering to provide higher accuracy. Experiments show that the LED with a spectrum width of about 50 nm has a lower limitation error than the laser and can achieve up to 58.1601 μm with focal length 200 mm and slit width 15 mm.

Direct single-shot phase retrieval from the diffraction pattern of separated objects

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

Leshem, Ben; Xu, Rui; Dallal, Yehonatan

The non-crystallographic phase problem arises in numerous scientific and technological fields. An important application is coherent diffractive imaging. Recent advances in X-ray free-electron lasers allow capturing of the diffraction pattern from a single nanoparticle before it disintegrates, in so-called ‘diffraction before destruction’ experiments. Presently, the phase is reconstructed by iterative algorithms, imposing a non-convex computational challenge, or by Fourier holography, requiring a well-characterized reference field. Here we present a convex scheme for single-shot phase retrieval for two (or more) sufficiently separated objects, demonstrated in two dimensions. In our approach, the objects serve as unknown references to one another, reducing themore » phase problem to a solvable set of linear equations. We establish our method numerically and experimentally in the optical domain and demonstrate a proof-of-principle single-shot coherent diffractive imaging using X-ray free-electron lasers pulses. Lastly, our scheme alleviates several limitations of current methods, offering a new pathway towards direct reconstruction of complex objects.« less

Direct single-shot phase retrieval from the diffraction pattern of separated objects

DOE PAGES

Leshem, Ben; Xu, Rui; Dallal, Yehonatan; ...

2016-02-22

The non-crystallographic phase problem arises in numerous scientific and technological fields. An important application is coherent diffractive imaging. Recent advances in X-ray free-electron lasers allow capturing of the diffraction pattern from a single nanoparticle before it disintegrates, in so-called ‘diffraction before destruction’ experiments. Presently, the phase is reconstructed by iterative algorithms, imposing a non-convex computational challenge, or by Fourier holography, requiring a well-characterized reference field. Here we present a convex scheme for single-shot phase retrieval for two (or more) sufficiently separated objects, demonstrated in two dimensions. In our approach, the objects serve as unknown references to one another, reducing themore » phase problem to a solvable set of linear equations. We establish our method numerically and experimentally in the optical domain and demonstrate a proof-of-principle single-shot coherent diffractive imaging using X-ray free-electron lasers pulses. Lastly, our scheme alleviates several limitations of current methods, offering a new pathway towards direct reconstruction of complex objects.« less

Diffracted light from latent images in photoresist for exposure control

DOEpatents

Bishop, Kenneth P.; Brueck, Steven R. J.; Gaspar, Susan M.; Hickman, Kirt C.; McNeil, John R.; Naqvi, S. Sohail H.; Stallard, Brian R.; Tipton, Gary D.

1997-01-01

In microelectronics manufacturing, an arrangement for monitoring and control of exposure of an undeveloped photosensitive layer on a structure susceptible to variations in optical properties in order to attain the desired critical dimension for the pattern to be developed in the photosensitive layer. This is done by ascertaining the intensities for one or more respective orders of diffracted power for an incident beam of radiation corresponding to the desired critical dimension for the photosensitive layer as a function of exposure time and optical properties of the structure, illuminating the photosensitive layer with a beam of radiation of one or more frequencies to which the photosensitive layer is not exposure-sensitive, and monitoring the intensities of the orders of diffracted radiation due to said illumination including at least the first order of diffracted radiation thereof, such that when said predetermined intensities for the diffracted orders are reached during said illumination of photosensitive layer, it is known that a pattern having at least approximately the desired critical dimension can be developed on the photosensitive layer.

Large-Scale Diffraction Patterns from Circular Objects

ERIC Educational Resources Information Center

Rinard, Phillip M.

1976-01-01

Investigates quantitatively the diffractions of light by a U.S. penny and an aperture of the same size. Differences noted between the theory and measurements are discussed, with probable causes indicated. (Author/CP)

Three-dimensional nanostructure determination from a large diffraction data set recorded using scanning electron nanodiffraction.

PubMed

Meng, Yifei; Zuo, Jian-Min

2016-09-01

A diffraction-based technique is developed for the determination of three-dimensional nanostructures. The technique employs high-resolution and low-dose scanning electron nanodiffraction (SEND) to acquire three-dimensional diffraction patterns, with the help of a special sample holder for large-angle rotation. Grains are identified in three-dimensional space based on crystal orientation and on reconstructed dark-field images from the recorded diffraction patterns. Application to a nanocrystalline TiN thin film shows that the three-dimensional morphology of columnar TiN grains of tens of nanometres in diameter can be reconstructed using an algebraic iterative algorithm under specified prior conditions, together with their crystallographic orientations. The principles can be extended to multiphase nanocrystalline materials as well. Thus, the tomographic SEND technique provides an effective and adaptive way of determining three-dimensional nanostructures.

Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

PubMed Central

Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

2018-01-01

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

Broadband diffractive lens or imaging element

DOEpatents

Ceglio, Natale M.; Hawryluk, Andrew M.; London, Richard A.; Seppala, Lynn G.

1991-01-01

A broadband diffractive lens or imaging element produces a sharp focus and/or a high resolution image with broad bandwidth illuminating radiation. The diffractive lens is sectored or segmented into regions, each of which focuses or images a distinct narrowband of radiation but all of which have a common focal length. Alternatively, a serial stack of minus filters, each with a diffraction pattern which focuses or images a distinct narrowband of radiation but all of which have a common focal length, is used. The two approaches can be combined. Multifocal broadband diffractive elements can also be formed.

Pattern formation without diffraction matching in optical parametric oscillators with a metamaterial.

PubMed

Tassin, Philippe; Van der Sande, Guy; Veretennicoff, Irina; Kockaert, Pascal; Tlidi, Mustapha

2009-05-25

We consider a degenerate optical parametric oscillator containing a left-handed material. We show that the inclusion of a left-handed material layer allows for controlling the strength and sign of the diffraction coefficient at either the pump or the signal frequency. Subsequently, we demonstrate the existence of stable dissipative structures without diffraction matching, i.e., without the usual relationship between the diffraction coefficients of the signal and pump fields. Finally, we investigate the size scaling of these light structures with decreasing diffraction strength.

Study of ZnO and Mg doped ZnO nanoparticles by sol-gel process

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

Ansari, Mohd Meenhaz, E-mail: meenhazphysics@gmail.com; Arshad, Mohd; Tripathi, Pushpendra

Nano-crystalline undoped and Mg doped ZnO (Mg-ZnO) nanoparticles with compositional formula Mg{sub x}Zn{sub 1-x}O (x=0,1,3,5,7,10 and 12 %) were synthesized using sol-gel process. The XRD diffraction peaks match with the pattern of the standard hexagonal structure of ZnO that reveals the formation of hexagonal wurtzite structure in all samples. SEM images demonstrates clearly the formation of spherical ZnO nanoparticles, and change of the morphology of the nanoparticles with the concentration of the magnesium, which is in close agreement with that estimated by Scherer formula based on the XRD pattern. To investigate the doping effect on optical properties, the UV–VIS absorptionmore » spectra was obtained and the band gap of the samples calculated.« less

Disparities in correlating microstructural to nanostructural preservation of dinosaur femoral bones

NASA Astrophysics Data System (ADS)

Kim, Jung-Kyun; Kwon, Yong-Eun; Lee, Sang-Gil; Lee, Ji-Hyun; Kim, Jin-Gyu; Huh, Min; Lee, Eunji; Kim, Youn-Joong

2017-03-01

Osteohistological researches on dinosaurs are well documented, but descriptions of direct correlations between the bone microstructure and corresponding nanostructure are currently lacking. By applying correlative microscopy, we aimed to verify that well-preserved osteohistological features correlate with pristine fossil bone nanostructures from the femoral bones of Koreanosaurus boseongensis. The quality of nanostructural preservation was evaluated based on the preferred orientation level of apatite crystals obtained from selected area electron diffraction (SAED) patterns and by measuring the “arcs” from the {100} and {002} diffraction rings. Unlike our expectations, our results revealed that well-preserved microstructures do not guarantee pristine nanostructures and vice versa. Structural preservation of bone from macro- to nanoscale primarily depends on original bioapatite density, and subsequent taphonomical factors such as effects from burial, pressure, influx of external elements and the rate of diagenetic alteration of apatite crystals. Our findings suggest that the efficient application of SAED analysis opens the opportunity for comprehensive nanostructural investigations of bone.

Synthesis of ZnSnO{sub 3} nanostructure by sol gel method

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

Para, Touseef Ahmad; Reshi, Hilal Ahmad; Shelke, Vilas, E-mail: drshelke@gmail.com

2016-05-23

Zinc Stannate (ZST) with composition ZnSnO{sub 3} is known for high electron mobility, optical, piezoelectric and charge storage properties. ZST crystalizes in different lattice structures, which allows a wide range of tunablity. We demonstrate successful synthesis of ZnSnO{sub 3} nanomaterial by sol-gel method. ZnSnO{sub 3} nanomaterials were calcined and sintered at different temperatures. Powder X-ray diffraction confirmed the single phase of the nanomaterial with rhombohedral R-3 space group. The Rietveld refinement of diffraction pattern yielded lattice parameter values a=5.26Å, c=14.09Å. Raman spectroscopy revealed higher activity towards higher wavenumbers. Raman shift around 530cm{sup −1} was found to be highly structure dependent,more » most probably due to anharmonic atomic vibrations in ZnO{sub 6}/SnO{sub 6} octahedra around center of mass. Sharp Peak around 650cm{sup −1} is characteristic of ZnSnO{sub 3} molecule.« less

Microscopic modulation of mechanical properties in transparent insect wings

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

Arora, Ashima; Kumar, Pramod; Bhagavathi, Jithin

We report on the measurement of local friction and adhesion of transparent insect wings using an atomic force microscope cantilever down to nanometre length scales. We observe that the wing-surface is decorated with 10 μm long and 2 μm wide islands that have higher topographic height. The friction on the islands is two orders of magnitude higher than the back-ground while the adhesion on the islands is smaller. Furthermore, the high islands are decorated with ordered nano-wire-like structures while the background is full of randomly distributed granular nano-particles. Coherent optical diffraction through the wings produce a stable diffraction pattern revealing a quasi-periodicmore » organization of the high islands over the entire wing. This suggests a long-range order in the modulation of friction and adhesion which is directly correlated with the topography. The measurements unravel novel functional design of complex wing surface and could find application in miniature biomimetic devices.« less

Quantification of thickness and wrinkling of exfoliated two-dimensional zeolite nanosheets

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

Kumar, Prashant; Agrawal, Kumar Varoon; Tsapatsis, Michael

Some two-dimensional (2D) exfoliated zeolites are single- or near single-unit cell thick silicates that can function as molecular sieves. Although they have already found uses as catalysts, adsorbents and membranes precise determination of their thickness and wrinkling is critical as these properties influence their functionality. Here we demonstrate a method to accurately determine the thickness and wrinkles of a 2D zeolite nanosheet by comprehensive 3D mapping of its reciprocal lattice. Since the intensity modulation of a diffraction spot on tilting is a fingerprint of the thickness, and changes in the spot shape are a measure of wrinkling, this mapping ismore » achieved using a large-angle tilt-series of electron diffraction patterns. As a result, application of the method to a 2D zeolite with MFI structure reveals that the exfoliated MFI nanosheet is 1.5 unit cells (3.0 nm) thick and wrinkled anisotropically with up to 0.8 nm average surface roughness.« less

Ultrafast atomic-scale visualization of acoustic phonons generated by optically excited quantum dots

PubMed Central

Vanacore, Giovanni M.; Hu, Jianbo; Liang, Wenxi; Bietti, Sergio; Sanguinetti, Stefano; Carbone, Fabrizio; Zewail, Ahmed H.

2017-01-01

Understanding the dynamics of atomic vibrations confined in quasi-zero dimensional systems is crucial from both a fundamental point-of-view and a technological perspective. Using ultrafast electron diffraction, we monitored the lattice dynamics of GaAs quantum dots—grown by Droplet Epitaxy on AlGaAs—with sub-picosecond and sub-picometer resolutions. An ultrafast laser pulse nearly resonantly excites a confined exciton, which efficiently couples to high-energy acoustic phonons through the deformation potential mechanism. The transient behavior of the measured diffraction pattern reveals the nonequilibrium phonon dynamics both within the dots and in the region surrounding them. The experimental results are interpreted within the theoretical framework of a non-Markovian decoherence, according to which the optical excitation creates a localized polaron within the dot and a travelling phonon wavepacket that leaves the dot at the speed of sound. These findings indicate that integration of a phononic emitter in opto-electronic devices based on quantum dots for controlled communication processes can be fundamentally feasible. PMID:28852685

Quantification of thickness and wrinkling of exfoliated two-dimensional zeolite nanosheets

DOE PAGES

Kumar, Prashant; Agrawal, Kumar Varoon; Tsapatsis, Michael; ...

2015-05-11

Some two-dimensional (2D) exfoliated zeolites are single- or near single-unit cell thick silicates that can function as molecular sieves. Although they have already found uses as catalysts, adsorbents and membranes precise determination of their thickness and wrinkling is critical as these properties influence their functionality. Here we demonstrate a method to accurately determine the thickness and wrinkles of a 2D zeolite nanosheet by comprehensive 3D mapping of its reciprocal lattice. Since the intensity modulation of a diffraction spot on tilting is a fingerprint of the thickness, and changes in the spot shape are a measure of wrinkling, this mapping ismore » achieved using a large-angle tilt-series of electron diffraction patterns. As a result, application of the method to a 2D zeolite with MFI structure reveals that the exfoliated MFI nanosheet is 1.5 unit cells (3.0 nm) thick and wrinkled anisotropically with up to 0.8 nm average surface roughness.« less

Gas-phase surface esterification of cellulose microfibrils and whiskers.

PubMed

Berlioz, Sophie; Molina-Boisseau, Sonia; Nishiyama, Yoshiharu; Heux, Laurent

2009-08-10

A new and highly efficient synthetic method has been developed for the surface esterification of model cellulosic substrates of high crystallinity and accessibility, namely, freeze-dried tunicin whiskers and bacterial cellulose microfibrils dried by the critical point method. The reaction, which is based on the gas-phase action of palmitoyl chloride, was monitored by solid-state CP-MAS (13)C NMR. It was found that the grafting density not only depended on the experimental conditions, but also on the nature and conditioning of the cellulose samples. The structural and morphological modifications of the substrates at various degrees of grafting were revealed by scanning electron microscopy and X-ray diffraction analysis. These characterizations indicated that the esterification proceeded from the surface of the substrate to their crystalline core. Hence, for moderate degree of substitution, the surface was fully grafted whereas the cellulose core remained unmodified and the original fibrous morphology maintained. An almost total esterification could be achieved under certain conditions, leading to highly substituted cellulose esters, presenting characteristic X-ray diffraction patterns.

Three-dimensional silicon inverse photonic quasicrystals for infrared wavelengths.

PubMed

Ledermann, Alexandra; Cademartiri, Ludovico; Hermatschweiler, Martin; Toninelli, Costanza; Ozin, Geoffrey A; Wiersma, Diederik S; Wegener, Martin; von Freymann, Georg

2006-12-01

Quasicrystals are a class of lattices characterized by a lack of translational symmetry. Nevertheless, the points of the lattice are deterministically arranged, obeying rotational symmetry. Thus, we expect properties that are different from both crystals and glasses. Indeed, naturally occurring electronic quasicrystals (for example, AlPdMn metal alloys) show peculiar electronic, vibrational and physico-chemical properties. Regarding artificial quasicrystals for electromagnetic waves, three-dimensional (3D) structures have recently been realized at GHz frequencies and 2D structures have been reported for the near-infrared region. Here, we report on the first fabrication and characterization of 3D quasicrystals for infrared frequencies. Using direct laser writing combined with a silicon inversion procedure, we achieve high-quality silicon inverse icosahedral structures. Both polymeric and silicon quasicrystals are characterized by means of electron microscopy and visible-light Laue diffraction. The diffraction patterns of structures with a local five-fold real-space symmetry axis reveal a ten-fold symmetry as required by theory for 3D structures.

Atomic electric fields revealed by a quantum mechanical approach to electron picodiffraction.

PubMed

Müller, Knut; Krause, Florian F; Béché, Armand; Schowalter, Marco; Galioit, Vincent; Löffler, Stefan; Verbeeck, Johan; Zweck, Josef; Schattschneider, Peter; Rosenauer, Andreas

2014-12-15

By focusing electrons on probes with a diameter of 50 pm, aberration-corrected scanning transmission electron microscopy (STEM) is currently crossing the border to probing subatomic details. A major challenge is the measurement of atomic electric fields using differential phase contrast (DPC) microscopy, traditionally exploiting the concept of a field-induced shift of diffraction patterns. Here we present a simplified quantum theoretical interpretation of DPC. This enables us to calculate the momentum transferred to the STEM probe from diffracted intensities recorded on a pixel array instead of conventional segmented bright-field detectors. The methodical development yielding atomic electric field, charge and electron density is performed using simulations for binary GaN as an ideal model system. We then present a detailed experimental study of SrTiO3 yielding atomic electric fields, validated by comprehensive simulations. With this interpretation and upgraded instrumentation, STEM is capable of quantifying atomic electric fields and high-contrast imaging of light atoms.

Atomic electric fields revealed by a quantum mechanical approach to electron picodiffraction

NASA Astrophysics Data System (ADS)

Müller, Knut; Krause, Florian F.; Béché, Armand; Schowalter, Marco; Galioit, Vincent; Löffler, Stefan; Verbeeck, Johan; Zweck, Josef; Schattschneider, Peter; Rosenauer, Andreas

2014-12-01

By focusing electrons on probes with a diameter of 50 pm, aberration-corrected scanning transmission electron microscopy (STEM) is currently crossing the border to probing subatomic details. A major challenge is the measurement of atomic electric fields using differential phase contrast (DPC) microscopy, traditionally exploiting the concept of a field-induced shift of diffraction patterns. Here we present a simplified quantum theoretical interpretation of DPC. This enables us to calculate the momentum transferred to the STEM probe from diffracted intensities recorded on a pixel array instead of conventional segmented bright-field detectors. The methodical development yielding atomic electric field, charge and electron density is performed using simulations for binary GaN as an ideal model system. We then present a detailed experimental study of SrTiO3 yielding atomic electric fields, validated by comprehensive simulations. With this interpretation and upgraded instrumentation, STEM is capable of quantifying atomic electric fields and high-contrast imaging of light atoms.

Atomic electric fields revealed by a quantum mechanical approach to electron picodiffraction

PubMed Central

Müller, Knut; Krause, Florian F.; Béché, Armand; Schowalter, Marco; Galioit, Vincent; Löffler, Stefan; Verbeeck, Johan; Zweck, Josef; Schattschneider, Peter; Rosenauer, Andreas

2014-01-01

By focusing electrons on probes with a diameter of 50 pm, aberration-corrected scanning transmission electron microscopy (STEM) is currently crossing the border to probing subatomic details. A major challenge is the measurement of atomic electric fields using differential phase contrast (DPC) microscopy, traditionally exploiting the concept of a field-induced shift of diffraction patterns. Here we present a simplified quantum theoretical interpretation of DPC. This enables us to calculate the momentum transferred to the STEM probe from diffracted intensities recorded on a pixel array instead of conventional segmented bright-field detectors. The methodical development yielding atomic electric field, charge and electron density is performed using simulations for binary GaN as an ideal model system. We then present a detailed experimental study of SrTiO3 yielding atomic electric fields, validated by comprehensive simulations. With this interpretation and upgraded instrumentation, STEM is capable of quantifying atomic electric fields and high-contrast imaging of light atoms. PMID:25501385

Computational prediction of body-centered cubic carbon in an all- s p 3 six-member ring configuration

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

Li, Zhen -Zhen; Lian, Chao -Sheng; Xu, Jing

2015-06-11

Recent shock compression experiments produced clear evidence of a new carbon phase, but a full structural identification has remained elusive. Here we establish by ab initio calculations a body-centered cubic carbon phase in Ia3¯d(O 10 h) symmetry, which contains twelve atoms in its primitive cell, thus termed BC12, and comprises all-sp 3 six-membered rings. This structural configuration places BC12 carbon in the same bonding type as cubic diamond, and its stability is verified by phonon mode analysis. Simulated x-ray diffraction patterns provide an excellent match to the previously unexplained distinct diffraction peak found in shock compression experiments. Electronic band andmore » density of states calculations reveal that BC12 is a semiconductor with a direct band gap of ~2.97eV. Lastly, these results provide a solid foundation for further exploration of this new carbon allotrope.« less

High-resolution inelastic neutron scattering and neutron powder diffraction study of the adsorption of dihydrogen by the Cu(II) metal-organic framework material HKUST-1

NASA Astrophysics Data System (ADS)

Callear, Samantha K.; Ramirez-Cuesta, Anibal J.; David, William I. F.; Millange, Franck; Walton, Richard I.

2013-12-01

We present new high-resolution inelastic neutron scattering (INS) spectra (measured using the TOSCA and MARI instruments at ISIS) and powder neutron diffraction data (measured on the diffractometer WISH at ISIS) from the interaction of the prototypical metal-organic framework HKUST-1 with various dosages of dihydrogen gas. The INS spectra show direct evidence for the sequential occupation of various distinct sites for dihydrogen in the metal-organic framework, whose population is adjusted during increasing loading of the guest. The superior resolution of TOSCA reveals subtle features in the spectra, not previously reported, including evidence for split signals, while complementary spectra recorded on MARI present full information in energy and momentum transfer. The analysis of the powder neutron patterns using the Rietveld method shows a consistent picture, allowing the crystallographic indenisation of binding sites for dihydrogen, thus building a comprehensive picture of the interaction of the guest with the nanoporous host.

Modified alignment CGHs for aspheric surface test

NASA Astrophysics Data System (ADS)

Song, Jae-Bong; Yang, Ho-Soon; Rhee, Hyug-Gyo; Lee, Yun-Woo

2009-08-01

Computer Generated Holograms (CGH) for optical test are commonly consisted of one main pattern for testing aspheric surface and some alignment patterns for aligning the interferometer, CGH, and the test optics. To align the CGH plate and the test optics, we designed the alignment CGHs modified from the cat's eye alignment method, which are consisted of a couple of CGH patterns. The incident beam passed through the one part of the alignment CGH pattern is focused onto the one radius position of the test aspheric surface, and is reflected to the other part, and vice versa. This method has several merits compared to the conventional cat's eye alignment method. First, this method can be used in testing optics with a center hole, and the center part of CGH plate can be assigned to the alignment pattern. Second, the alignment pattern becomes a concentric circular arc pattern. The whole CGH patterns including the main pattern and alignment patterns are consisted of only concentric circular fringes. This concentric circular pattern can be easily made by the polar coordinated writer with circular scanning. The required diffraction angle becomes relatively small, so the 1st order diffraction beams instead of the 3rd order diffraction beam can be used as alignment beams, and the visibility can be improved. This alignment method also is more sensitive to the tilt and the lateral shift of the test aspheric surface. Using this alignment pattern, a 200 mm diameter F/0.5 aspheric mirror and a 600 mm diameter F/0.9 mirror were tested.

Structures of Astromaterials Revealed by EBSD

NASA Technical Reports Server (NTRS)

Zolensky, M.

2018-01-01

Groups at the Johnson Space Center and the University of Tokyo have been using electron back-scattered diffraction (EBSD) to reveal the crystal structures of extraterrestrial minerals for many years. Even though we also routinely use transmission electron microscopy, synchrotron X-ray diffraction (SXRD), and conventional electron diffraction, we find that EBSD is the most powerful technique for crystal structure elucidation in many instances. In this talk I describe a few of the cases where we have found EBSD to provide crucial, unique information. See attachment.

Structure investigations of ferromagnetic Co-Ni-Al alloys obtained by powder metallurgy.

PubMed

Maziarz, W; Dutkiewicz, J; Lityńska-Dobrzyńska, L; Santamarta, R; Cesari, E

2010-03-01

Elemental powders of Co, Ni and Al in the proper amounts to obtain Co(35)Ni(40)Al(25) and Co(40)Ni(35)Al(25) nominal compositions were ball milled in a high-energy mill for 80 h. After 40 h of milling, the formation of a Co (Ni, Al) solid solution with f.c.c. structure was verified by a change of the original lattice parameter and crystallite size. Analytical transmission electron microscopy observations and X-ray diffraction measurements of the final Co (Ni, Al) solid solution showed that the crystallite size scattered from 4 to 8 nm and lattice parameter a = 0.36086 nm. The chemical EDS point analysis of the milled powder particles allowed the calculation of the e/a ratio and revealed a high degree of chemical homogeneity of the powders. Hot pressing in vacuum of the milled powders resulted in obtaining compacts with a density of about 70% of the theoretical one. An additional heat treatment increased the density and induced the martensitic transformation in a parent phase. Selected area diffraction patterns and dark field images obtained from the heat-treated sample revealed small grains around 300 nm in diameter consisting mainly of the ordered gamma phase (gamma'), often appearing as twins, and a small amount of the L1(0) ordered martensite.

Microstructural, Magnetic, and Optical Properties of Pr-Doped Perovskite Manganite La0.67Ca0.33MnO3 Nanoparticles Synthesized via Sol-Gel Process

NASA Astrophysics Data System (ADS)

Xia, Weiren; Wu, Heng; Xue, Piaojie; Zhu, Xinhua

2018-05-01

We report on microstructural, magnetic, and optical properties of Pr-doped perovskite manganite (La1 - xPrx)0.67Ca0.33MnO3 (LPCMO, x = 0.0-0.5) nanoparticles synthesized via sol-gel process. Structural characterizations (X-ray and electron diffraction patterns, (high resolution) TEM images) provide information regarding the phase formation and the single-crystalline nature of the LPCMO systems. X-ray and electron diffraction patterns reveal that all the LPCMO samples crystallize in perovskite crystallography with an orthorhombic structure ( Pnma space group), where the MnO6 octahedron is elongated along the b axis due to the Jahn-Teller effect. That is confirmed by Raman spectra. Crystallite sizes and grain sizes were calculated from XRD and TEM respectively, and the lattice fringes resolved in the high-resolution TEM images of individual LPCMO nanoparticle confirmed its single-crystalline nature. FTIR spectra identify the characteristic Mn-O bond stretching vibration mode near 600 cm- 1, which shifts towards high wavenumbers with increasing post-annealing temperature or Pr-doping concentration, resulting in further distortion of the MnO6 octahedron. XPS revealed dual oxidation states of Mn3+ and Mn4+ in the LPCMO nanoparticles. UV-vis absorption spectra confirm the semiconducting nature of the LPCMO nanoparticles with optical bandgaps of 2.55-2.71 eV. Magnetic measurements as a function of temperature and magnetic field at field cooling and zero-field cooling modes, provided a Curie temperature around 230 K, saturation magnetization of about 81 emu/g, and coercive field of 390 Oe at 10 K. Such magnetic properties and the semiconducting nature of the LPCMO nanoparticles will make them as suitable candidate for magnetic semiconductor spintronics.

Comments on the paper "Bragg's law diffraction simulations for electron backscatter diffraction analysis" by Josh Kacher, Colin Landon, Brent L. Adams & David Fullwood.

PubMed

Maurice, Claire; Fortunier, Roland; Driver, Julian; Day, Austin; Mingard, Ken; Meaden, Graham

2010-06-01

This comment on the paper "Bragg's Law diffraction simulations for electron backscatter diffraction analysis" by Kacher et al. explains the limitations in determining elastic strains using synthetic EBSD patterns. Of particular importance are those due to the accuracy of determination of the EBSD geometry projection parameters. Additional references and supporting information are provided. Copyright 2010 Elsevier B.V. All rights reserved.

Étude de la structure des alliages vitreux Ag-As2S3 par diffraction de rayons X

NASA Astrophysics Data System (ADS)

Popescu, M.; Sava, F.; Cornet, A.; Broll, N.

2002-07-01

The structure of several silver alloyed arsenic chalocgenide has been determined by X-ray diffraction. For low silver doping the disordered layer structure, characteristic to the glassy AS2S3 is retained as demonstrated by the well developed first sharp diffraction peak in the X-ray diffraction pattern. For high amount of silver introduced in the As2S3 matrix, the disoredered layer configurations disappear, as shown by the diminishing and even disappearance of the first sharp diffraction peak in the X-ray patterns. A three-dimensional structure based on Ag2S -type configuration is formed. La structure de quelques alliages sulfure d'arsenic - argent a été determinée par diffraction de rayons X. Pour de faibles dopages à l'argent on conserve la structure desordonnées caractéristique des couches atomique d'As2S3 vitreux ; ceci est prouvé par la forte intensité du premier pic étroit de diffraction. Pour des plus grandes proportions d'argent la structure de l'alliage vitreux fait apparaître des unités structurales caractéristiques du cristal d'Ag2S et la configuration atomique avec des couches desordonnées disparaît (le premier pic étroit de diffraction s'évanouit) en faisant place à une structure tridimensionelle.

Continuous diffraction of molecules and disordered molecular crystals

PubMed Central

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

2017-01-01

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

Development of splitting convergent beam electron diffraction (SCBED).

PubMed

Houdellier, Florent; Röder, Falk; Snoeck, Etienne

2015-12-01

Using a combination of condenser electrostatic biprism with dedicated electron optic conditions for sample illumination, we were able to split a convergent beam electron probe focused on the sample in two half focused probes without introducing any tilt between them. As a consequence, a combined convergent beam electron diffraction pattern is obtained in the back focal plane of the objective lens arising from two different sample areas, which could be analyzed in a single pattern. This splitting convergent beam electron diffraction (SCBED) pattern has been tested first on a well-characterized test sample of Si/SiGe multilayers epitaxially grown on a Si substrate. The SCBED pattern contains information from the strained area, which exhibits HOLZ lines broadening induced by surface relaxation, with fine HOLZ lines observed in the unstrained reference part of the sample. These patterns have been analyzed quantitatively using both parts of the SCBED transmitted disk. The fine HOLZ line positions are used to determine the precise acceleration voltage of the microscope while the perturbed HOLZ rocking curves in the stained area are compared to dynamical simulated ones. The combination of these two information leads to a precise evaluation of the sample strain state. Finally, several SCBED setups are proposed to tackle fundamental physics questions as well as applied materials science ones and demonstrate how SCBED has the potential to greatly expand the range of applications of electron diffraction and electron holography. Copyright © 2015 Elsevier B.V. All rights reserved.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE PAGES

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; ...

2015-08-11

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary tomore » fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15µm) loaded into the chips yielded a complete, high-resolution (<1.6Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

PubMed Central

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

2015-01-01

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs. PMID:26457423

Diffractive Optic Fluid Shear Stress Sensor

NASA Technical Reports Server (NTRS)

Wilson, D.; Scalf, J.; Forouhar, S.; Muller, R.; Taugwalder, F.; Gharib, M.; Fourguette, D.; Modarress, D.

2000-01-01

Light scattering off particles flowing through a two-slit interference pattern can be used to measure the shear stress of the fluid. We have designed and fabricated a miniature diffractive optic sensor based on this principle.

Studies on X-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Miao, Huijie

This dissertation includes three main parts: studies on coherence requirements for the diffraction microscopy experiments, ice formation on frozen-hydrated sample during data collection, and centering of the diffraction data sets. These three subjects are all in support of our groups overall goal of high resolution 3D imaging of frozen hydrated eukaryotic cells via x-ray diffraction microscopy. X-ray diffraction microscopy requires coherent illumination. However, the actual degree of coherence at some beamlines has never been tested. In research on coherence, our first aim is to determine the transverse coherence width at the sample plane at BL 9.0.1 at the Advanced Light Source in Lawrence Berkeley National Laboratory. An analytical calculation of the coherence at the sample plane is presented. Experimental diffraction patterns of pinhole-pair samples were also taken at the beamline to determine the coherence. Due to the irregular shape of the pinholes and other optics complexity, it was very difficult to fit the data with known theoretical equations as it was traditionally done with 1D data. However, we found out that the auto-correlation function shows clearly three spots. Theoretical calculation have been carried out to show that the degree of coherence can be obtained from the intensities of the three spots. These results are compared with the results from the analytical calculation. We then perform a simulation, showing the required transverse coherence width for reconstructing samples with a given size. Ice accumulation has been a major problem in X-ray diffraction microscopy with frozen hydrated samples. Since the ice structure is different from point to point, we cannot subtract the scattering from ice, nor assume a completely "empty" region outside the finite support constraint area as required for reconstruction. Ice forms during the sample preparation and transfer. However, from the tests we did in September 2007, we found that the ice layer thickens significantly during the data collecting process. One of the tests we did was putting a dry room-temperature grid into the beam, cooling it down to liquid nitrogen temperature, and then collecting the diffraction pattern of it over time. This test showed that, after the cold grid remained in the chamber for a while, a ring could be observed in the diffraction pattern. The time necessary for this ring to be visible is highly dependent on the pressure and vacuum history of the chamber. We will discuss how the chamber pressure influences the ice accumulation rate, how an anti-contamination device can help to reduce the rate, and how this ring forms. The last part of the research is based on simulations and a real data set collected on beamline 9.0.1 at the ALS in Berkeley. In X-ray diffraction microscopy, one of the major challenges when processing the data is to accurately determine the true center of the recorded data; that is, the zero spatial frequency position. Simulations of reconstructing shifted data show that if the center of a 2D diffraction pattern is shifted by more than 3 pixels from its true center, the positivity constraint to the phase, which otherwise might be applied to improve the convergence of the reconstruction algorithm, cannot be imposed. Moreover, the phase unwrapping problem may appear during the reconstruction. These issues undermine the quality of the reconstruction of 2D data. Furthermore, the individual shift in each 2D pattern will lead to errors when assembling a 3D diffraction data cube, making the 3D reconstruction very difficult. We developed a method which uses power spectra of the partial diffraction pattern to pre-align the data. A reconstruction without severe phase unwrapping can then be obtained from the pre-aligned data. Next, the precise zero spatial frequency position can be found by examining the linear ramp present in the reconstructed phase. This method was applied to a freeze-dried yeast data set to show that this approach is effective with experimental data.

Anomalous refraction of light through slanted-nanoaperture arrays on metal surface

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

Kim, Myungji; Jung, Yun Suk; Xi, Yonggang

2015-09-07

We report a nanoapertured metal surface that demonstrates anomalous refraction of light for a wide range of incident angles. A nanoslit aperture is designed to serve as a tilted vertical-dipole whose radiation pattern orients to a glancing angle direction to substrate. An array of such slanted nanoslits formed in a metal film redirects an incident beam into the direction of negative refraction angle: the aperture-transmitted wave makes a far-field propagation to the tilt-oriented direction of radiation pattern. The thus-designed nanoaperture array demonstrates the −1st order diffraction (i.e., to the negative refraction-angle direction) with well-suppressed background transmission (the zero-order direct transmissionmore » and other higher-order diffractions). Engineering the radiation pattern of nanoaperture offers an approach to overcoming the limits of conventional diffractive/refractive optics and complementing metasurface-based nano-optics.« less

Growth of high quality and large-sized Rb 0.3MoO 3 single crystals by molten salt electrolysis method

NASA Astrophysics Data System (ADS)

Wang, Junfeng; Xiong, Rui; Yi, Fan; Yin, Di; Ke, Manzhu; Li, Changzhen; Liu, Zhengyou; Shi, Jing

2005-05-01

High quality and large-sized Rb 0.3MoO 3 single crystals were synthesized by molten salt electrolysis method. X-ray diffraction (XRD) patterns and rocking curves, as well as the white beam Laue diffraction of X-ray images show the crystals grown by this method have high quality. The lattice constants evaluated from XRD patterns are a0=1.87 nm, b0=0.75 nm, c0=1.00 nm, β=118.83∘. The in situ selected area electron diffraction (SAED) patterns along the [101¯], [11¯1¯] and [103¯] zone axes at room temperature indicate that the Rb 0.3MoO 3 crystal possess perfect C-centered symmetry. Temperature dependence of the resistivity shows this compound undergoes a metal to semiconductor transition at 183 K.

Low-energy Auger electron diffraction: influence of multiple scattering and angular momentum

NASA Astrophysics Data System (ADS)

Chassé, A.; Niebergall, L.; Kucherenko, Yu.

2002-04-01

The angular dependence of Auger electrons excited from single-crystal surfaces is treated theoretically within a multiple-scattering cluster model taking into account the full Auger transition matrix elements. In particular the model has been used to discuss the influence of multiple scattering and angular momentum of the Auger electron wave on Auger electron diffraction (AED) patterns in the region of low kinetic energies. Theoretical results of AED patterns are shown and discussed in detail for Cu(0 0 1) and Ni(0 0 1) surfaces, respectively. Even though Cu and Ni are very similar in their electronic and scattering properties recently strong differences have been found in AED patterns measured in the low-energy region. It is shown that the differences may be caused to superposition of different electron diffraction effects in an energy-integrated experiment. A good agreement between available experimental and theoretical results has been achieved.

Fourier phase retrieval with a single mask by Douglas-Rachford algorithms.

PubMed

Chen, Pengwen; Fannjiang, Albert

2018-05-01

The Fourier-domain Douglas-Rachford (FDR) algorithm is analyzed for phase retrieval with a single random mask. Since the uniqueness of phase retrieval solution requires more than a single oversampled coded diffraction pattern, the extra information is imposed in either of the following forms: 1) the sector condition on the object; 2) another oversampled diffraction pattern, coded or uncoded. For both settings, the uniqueness of projected fixed point is proved and for setting 2) the local, geometric convergence is derived with a rate given by a spectral gap condition. Numerical experiments demonstrate global, power-law convergence of FDR from arbitrary initialization for both settings as well as for 3 or more coded diffraction patterns without oversampling. In practice, the geometric convergence can be recovered from the power-law regime by a simple projection trick, resulting in highly accurate reconstruction from generic initialization.

Observation of ‘hidden’ planar defects in boron carbide nanowires and identification of their orientations

PubMed Central

2014-01-01

The physical properties of nanostructures strongly depend on their structures, and planar defects in particular could significantly affect the behavior of the nanowires. In this work, planar defects (twins or stacking faults) in boron carbide nanowires are extensively studied by transmission electron microscopy (TEM). Results show that these defects can easily be invisible, i.e., no presence of characteristic defect features like modulated contrast in high-resolution TEM images and streaks in diffraction patterns. The simplified reason of this invisibility is that the viewing direction during TEM examination is not parallel to the (001)-type planar defects. Due to the unique rhombohedral structure of boron carbide, planar defects are only distinctive when the viewing direction is along the axial or short diagonal directions ([100], [010], or 1¯10) within the (001) plane (in-zone condition). However, in most cases, these three characteristic directions are not parallel to the viewing direction when boron carbide nanowires are randomly dispersed on TEM grids. To identify fault orientations (transverse faults or axial faults) of those nanowires whose planar defects are not revealed by TEM, a new approach is developed based on the geometrical analysis between the projected preferred growth direction of a nanowire and specific diffraction spots from diffraction patterns recorded along the axial or short diagonal directions out of the (001) plane (off-zone condition). The approach greatly alleviates tedious TEM examination of the nanowire and helps to establish the reliable structure–property relations. Our study calls attention to researchers to be extremely careful when studying nanowires with potential planar defects by TEM. Understanding the true nature of planar defects is essential in tuning the properties of these nanostructures through manipulating their structures. PMID:24423258

Observation of 'hidden' planar defects in boron carbide nanowires and identification of their orientations.

PubMed

Guan, Zhe; Cao, Baobao; Yang, Yang; Jiang, Youfei; Li, Deyu; Xu, Terry T

2014-01-15

The physical properties of nanostructures strongly depend on their structures, and planar defects in particular could significantly affect the behavior of the nanowires. In this work, planar defects (twins or stacking faults) in boron carbide nanowires are extensively studied by transmission electron microscopy (TEM). Results show that these defects can easily be invisible, i.e., no presence of characteristic defect features like modulated contrast in high-resolution TEM images and streaks in diffraction patterns. The simplified reason of this invisibility is that the viewing direction during TEM examination is not parallel to the (001)-type planar defects. Due to the unique rhombohedral structure of boron carbide, planar defects are only distinctive when the viewing direction is along the axial or short diagonal directions ([100], [010], or 1¯10) within the (001) plane (in-zone condition). However, in most cases, these three characteristic directions are not parallel to the viewing direction when boron carbide nanowires are randomly dispersed on TEM grids. To identify fault orientations (transverse faults or axial faults) of those nanowires whose planar defects are not revealed by TEM, a new approach is developed based on the geometrical analysis between the projected preferred growth direction of a nanowire and specific diffraction spots from diffraction patterns recorded along the axial or short diagonal directions out of the (001) plane (off-zone condition). The approach greatly alleviates tedious TEM examination of the nanowire and helps to establish the reliable structure-property relations. Our study calls attention to researchers to be extremely careful when studying nanowires with potential planar defects by TEM. Understanding the true nature of planar defects is essential in tuning the properties of these nanostructures through manipulating their structures.

Molecular structure of self-assembled chiral nanoribbons and nanotubules revealed in the hydrated state.

PubMed

Oda, Reiko; Artzner, Franck; Laguerre, Michel; Huc, Ivan

2008-11-05

A detailed molecular organization of racemic 16-2-16 tartrate self-assembled multi-bilayer ribbons in the hydrated state is proposed where 16-2-16 amphiphiles, tartrate ions, and water molecules are all accurately positioned by comparing experimental X-ray powder diffraction and diffraction patterns derived from modeling studies. X-ray diffuse scattering studies show that molecular organization is not fundamentally altered when comparing the flat ribbons of the racemate to chirally twisted or helical ribbons of the pure tartrate enantiomer. Essential features of the three-dimensional molecular organizations of these structures include interdigitation of alkyl chains within each bilayer and well-defined networks of ionic and hydrogen bonds between cations, anions, and water molecules between bilayers. The detailed study of diffraction patterns also indicated that the gemini headgroups are oriented parallel to the long edge of the ribbons. The structure thus possesses a high cohesion and good crystallinity, and for the first time, we could relate the packing of the chiral molecules to the expression of the chirality at a mesoscopic scale. The organization of the ribbons at the molecular level sheds light on a number of their macroscopic features. Among these are the reason why enantiomerically pure 16-2-16 tartrate forms ribbons that consist of exactly two bilayers, and a plausible mechanism by which a chirally twisted or helical shape may emerge from the packing of chiral tartrate ions. Importantly, the distinction between commonly observed helical and twisted morphologies could be related to a subtle symmetry breaking. These results demonstrate that accurately solving the molecular structure of self-assembled soft materials--a process rarely achieved--is within reach, that it is a valid approach to correlate molecular parameters to macroscopic properties, and thus that it offers opportunities to modulate properties through molecular design.

Synthesis of silver nanoparticles by endosymbiont Pseudomonas fluorescens CA 417 and their bactericidal activity.

PubMed

Syed, Baker; M N, Nagendra Prasad; B L, Dhananjaya; K, Mohan Kumar; S, Yallappa; S, Satish

2016-12-01

The present study emphasizes on biogenic synthesis of silver nanoparticles and their bactericidal activity against human and phytopathogens. Nanoparticle synthesis was performed using endosymbiont Pseudomonas fluorescens CA 417 inhabiting Coffea arabica L. Synthesized nanoparticles were characterized using hyphenated spectroscopic techniques such as UV-vis spectroscopy which revealed maximum absorption 425nm. Fourier transform infrared spectroscopy (FTIR) analysis revealed the possible functional groups mediating and stabilizing silver nanoparticles with predominant peaks occurring at 3346 corresponding to hydroxyl group, 1635 corresponding carbonyl group and 680 to aromatic group. X-ray diffraction (XRD) analysis revealed the Bragg's diffraction pattern with distinct peaks at 38° 44°, 64° and 78° revealing the face-centered cubic (fcc) metallic crystal corresponding to the (111), (200), (220) and (311) facets of the crystal planes at 2θ angle. The energy dispersive X-ray spectroscopy (EDS) analysis revealed presence of high intense absorption peak at 3keV is a typical characteristic of nano-crystalline silver which confirmed the presence of elemental silver. TEM analysis revealed the size of the nanoparticles to be in the range 5-50nm with polydisperse nature of synthesized nanoparticles bearing myriad shapes. The particle size determined by Dynamic light scattering (DLS) method revealed average size to be 20.66nm. The synthesized silver nanoparticles exhibited significant antibacterial activity against panel of test pathogens. The results showed Klebsiella pneumoniae (MTCC 7407) and Xanthomonas campestris to be more sensitive among the test human pathogen and phyto-pathogen respectively. The study also reports synergistic effect of silver nanoparticles in combination with kanamycin which displayed increased fold activity up to 58.3% against Klebsiella pneumoniae (MTCC 7407). The results of the present investigation are promising enough and attribute towards growing scientific knowledge on development of new antimicrobial agents to combat drug resistant microorganisms. The study provides insight on emerging role of endophytes towards reduction of metal salts to synthesize nanoparticles. Copyright © 2016 Elsevier Inc. All rights reserved.

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.

Self-interferometric technique for visualization of phase patterns encoded onto a liquid-crystal display

NASA Astrophysics Data System (ADS)

Bentley, Joel B.; Davis, Jeffrey A.; Albero, Jorge; Moreno, Ignacio

2006-10-01

We report a new self-interferometric technique for visualizing phase patterns that are encoded onto a phase-only liquid-crystal display (LCD). In our approach, the LCD generates both the desired object beam as well as the reference beam. Normally the phase patterns are encoded with a phase depth of 2π radians, and all of the incident energy is diffracted into the first-order beam. However, by reducing this phase depth, we can generate an additional zero-order diffracted beam, which acts as the reference beam. We work at distances such that these two patterns spatially interfere, producing an interference pattern that displays the encoded phase pattern. This approach was used recently to display the phase vortices of helical Ince-Gaussian beams. Here we show additional experimental results and analyze the process.

X-Ray Diffraction and the Discovery of the Structure of DNA

ERIC Educational Resources Information Center

Crouse, David T.

2007-01-01

A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

Conical diffraction as a versatile building block to implement new imaging modalities for superresolution in fluorescence microscopy

NASA Astrophysics Data System (ADS)

Fallet, Clément; Caron, Julien; Oddos, Stephane; Tinevez, Jean-Yves; Moisan, Lionel; Sirat, Gabriel Y.; Braitbart, Philippe O.; Shorte, Spencer L.

2014-08-01

We present a new technology for super-resolution fluorescence imaging, based on conical diffraction. Conical diffraction is a linear, singular phenomenon taking place when a polarized beam is diffracted through a biaxial crystal. The illumination patterns generated by conical diffraction are more compact than the classical Gaussian beam; we use them to generate a super-resolution imaging modality. Conical Diffraction Microscopy (CODIM) resolution enhancement can be achieved with any type of objective on any kind of sample preparation and standard fluorophores. Conical diffraction can be used in multiple fashion to create new and disruptive technologies for super-resolution microscopy. This paper will focus on the first one that has been implemented and give a glimpse at what the future of microscopy using conical diffraction could be.

A helical biosonar scanning pattern in the Chinese noctule, Nyctalus plancyi.

PubMed

Müller, Rolf; Lu, Hongwang; Zhang, Shuyi; Peremans, Herbert

2006-06-01

Directivity and sound diffraction of the pinna of the Chinese Noctule (Nyctalus plancyi) have been studied numerically. The pinna was found capable of generating a periodic helical scanning pattern over frequency, if the tragus and the thickened lower ledge of the pinna rim were in an appropriate position. During the helical scan, a directivity pattern with a strong mainlobe alternated with a pattern dominated by a conical sleeve of sidelobes. This alternation was present, even when an unfavorable arrangement of the pinna disrupted the overall helical scanning pattern. In the fully formed helical scan, the orientation of main and sidelobes for different frequencies revealed a spatial ordering which extends volume coverage. Five different pinna parts have been removed from the digital pinna-shape representations in turn to assess their influence on the directivity. Of these parts, the tragus stem and the thickened lower ledge of the pinna rim were found to have the largest overall impact. The anatomical prominence of these structures was hence in agreement with their acoustic functionality. In the near-field, tragus stem and lower ledge were seen to act primarily through large shifts in the wavefield phase in both directions.

Low reflection and field localization over surface plasmon device with subwavelength patterned aluminum film

NASA Astrophysics Data System (ADS)

Yuan, Ying; Peng, Sha; Long, Huabao; Liu, Runhan; Wei, Dong; Zhang, Xinyu; Wang, Haiwei; Xie, Changsheng

2018-02-01

In this paper, we propose a new device composed of patterned sub-wavelength arrays to investigate surface plasmons (SPs) over sub-wavelength metal nano-structures. The device consists of silicon substrate and sub-wavelength patterns fabricated on a layer of aluminum film with nanometer thickness. Each sub-wavelength pattern formed in aluminum film is composed of a basic nano-square and twelve triangles for shaping single nano-pattern, which are uniformly distributed on the four sides of each square. Reflectance spectra and electric field distribution in infrared region are simulated. Numerical simulation results demonstrate that the device can efficiently lower its reflectance in infrared spectrum, and the response frequency can be controlled by only changing the device parameters such as square side length and then triangle vertex angle. Besides, the simulated electric field distribution of the device shows obviously field localization effect at the edges of aluminum film nano-structure. The electric filed around the tips of aluminum triangles is localized into sub-wavelength scale, so as to be beyond the common diffraction limitation. Our work will help to reveal the interesting properties of SPs device, and also bring new prospect of photonic device.

Three-dimensional nanostructure determination from a large diffraction data set recorded using scanning electron nanodiffraction

DOE PAGES

Meng, Yifei; Zuo, Jian -Min

2016-07-04

A diffraction-based technique is developed for the determination of three-dimensional nanostructures. The technique employs high-resolution and low-dose scanning electron nanodiffraction (SEND) to acquire three-dimensional diffraction patterns, with the help of a special sample holder for large-angle rotation. Grains are identified in three-dimensional space based on crystal orientation and on reconstructed dark-field images from the recorded diffraction patterns. Application to a nanocrystalline TiN thin film shows that the three-dimensional morphology of columnar TiN grains of tens of nanometres in diameter can be reconstructed using an algebraic iterative algorithm under specified prior conditions, together with their crystallographic orientations. The principles can bemore » extended to multiphase nanocrystalline materials as well. Furthermore, the tomographic SEND technique provides an effective and adaptive way of determining three-dimensional nanostructures.« less

Data preparation and evaluation techniques for x-ray diffraction microscopy

DOE PAGES

Steinbrener, Jan; Nelson, Johanna; Huang, Xiaojing; ...

2010-01-01

The post-experiment processing of X-ray Diffraction Microscopy data is often time-consuming and difficult. This is mostly due to the fact that even if a preliminary result has been reconstructed, there is no definitive answer as to whether or not a better result with more consistently retrieved phases can still be obtained. In addition, we show here that the first step in data analysis, the assembly of two-dimensional diffraction patterns from a large set of raw diffraction data, is crucial to obtaining reconstructions of highest possible consistency. We have developed software that automates this process and results in consistently accurate diffractionmore » patterns. We have furthermore derived some criteria of validity for a tool commonly used to assess the consistency of reconstructions, the phase retrieval transfer function, and suggest a modified version that has improved utility for judging reconstruction quality.« less

Exploring coherent electron excitation and migration dynamics by electron diffraction with ultrashort X-ray pulses.

PubMed

Yuan, Kai-Jun; Bandrauk, André D

2017-10-04

Exploring ultrafast charge migration is of great importance in biological and chemical reactions. We present a scheme to monitor attosecond charge migration in molecules by electron diffraction with spatial and temporal resolutions from ab initio numerical simulations. An ultraviolet pulse creates a coherent superposition of electronic states, after which a time-delayed attosecond X-ray pulse is used to ionize the molecule. It is found that diffraction patterns in the X-ray photoelectron spectra show an asymmetric structure, which is dependent on the time delay between the pump-probe pulses, encoding the information of molecular orbital symmetry and chemical bonding. We describe these phenomena by developing an electronic time-dependent ultrafast molecular photoionization model of a coherent superposition state. The periodical distortion of electron diffraction patterns illustrates the evolution of the electronic coherence, providing a tool for attosecond imaging of ultrafast molecular reaction processes.

A deep convolutional neural network to analyze position averaged convergent beam electron diffraction patterns.

PubMed

Xu, W; LeBeau, J M

2018-05-01

We establish a series of deep convolutional neural networks to automatically analyze position averaged convergent beam electron diffraction patterns. The networks first calibrate the zero-order disk size, center position, and rotation without the need for pretreating the data. With the aligned data, additional networks then measure the sample thickness and tilt. The performance of the network is explored as a function of a variety of variables including thickness, tilt, and dose. A methodology to explore the response of the neural network to various pattern features is also presented. Processing patterns at a rate of  ∼ 0.1 s/pattern, the network is shown to be orders of magnitude faster than a brute force method while maintaining accuracy. The approach is thus suitable for automatically processing big, 4D STEM data. We also discuss the generality of the method to other materials/orientations as well as a hybrid approach that combines the features of the neural network with least squares fitting for even more robust analysis. The source code is available at https://github.com/subangstrom/DeepDiffraction. Copyright © 2018 Elsevier B.V. All rights reserved.

Fatigue of LiNi0.8Co0.15Al0.05O2 in commercial Li ion batteries

NASA Astrophysics Data System (ADS)

Kleiner, Karin; Dixon, Ditty; Jakes, Peter; Melke, Julia; Yavuz, Murat; Roth, Christina; Nikolowski, Kristian; Liebau, Verena; Ehrenberg, Helmut

2015-01-01

The degradation of LiNi0.8Co0.15Al0.05O2 (LNCAO), a cathode material in lithium-ion-batteries, was studied using in situ powder diffraction and in situ Ni K edge X-ray absorption spectroscopy (XAS). The fatigued material was taken from a 7 Ah battery which was cycled for 34 weeks under defined durability conditions. Meanwhile, a cell was stored, as reference, under controlled conditions without electrochemical treatment. The fatigued LNCAO used in this study showed a capacity loss of 26% ± 9% compared to the non-cycled material. During charge and discharge the local and the overall structure of LNCAO was investigated by X-ray near edge structure (XANES) analysis, the extended X-ray absorption fine structure (EXAFS) analysis and by using Rietveld refinement of in situ powder diffraction patterns. Both powder diffraction and XAS revealed additional, rhombohedral phases which do not change with electrochemical cycling. Moreover, a phase with the lattice parameters of fully lithiated LNCAO was still present in the fatigued material at high potentials, while it was absent in the non-fatigued reference material. The coexistence of these phases is described by domains within the LNCAO particles, in correlation with the observed fatigue.

Coded diffraction system in X-ray crystallography using a boolean phase coded aperture approximation

NASA Astrophysics Data System (ADS)

Pinilla, Samuel; Poveda, Juan; Arguello, Henry

2018-03-01

Phase retrieval is a problem present in many applications such as optics, astronomical imaging, computational biology and X-ray crystallography. Recent work has shown that the phase can be better recovered when the acquisition architecture includes a coded aperture, which modulates the signal before diffraction, such that the underlying signal is recovered from coded diffraction patterns. Moreover, this type of modulation effect, before the diffraction operation, can be obtained using a phase coded aperture, just after the sample under study. However, a practical implementation of a phase coded aperture in an X-ray application is not feasible, because it is computationally modeled as a matrix with complex entries which requires changing the phase of the diffracted beams. In fact, changing the phase implies finding a material that allows to deviate the direction of an X-ray beam, which can considerably increase the implementation costs. Hence, this paper describes a low cost coded X-ray diffraction system based on block-unblock coded apertures that enables phase reconstruction. The proposed system approximates the phase coded aperture with a block-unblock coded aperture by using the detour-phase method. Moreover, the SAXS/WAXS X-ray crystallography software was used to simulate the diffraction patterns of a real crystal structure called Rhombic Dodecahedron. Additionally, several simulations were carried out to analyze the performance of block-unblock approximations in recovering the phase, using the simulated diffraction patterns. Furthermore, the quality of the reconstructions was measured in terms of the Peak Signal to Noise Ratio (PSNR). Results show that the performance of the block-unblock phase coded apertures approximation decreases at most 12.5% compared with the phase coded apertures. Moreover, the quality of the reconstructions using the boolean approximations is up to 2.5 dB of PSNR less with respect to the phase coded aperture reconstructions.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Johns Hopkins University School of Medicine, Baltimore, MD 21205; Lyubimov, Artem Y.

A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming themore » challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

Extraction and characterization of mixed phase KNO2-KNO3 nanocrystals derived from flat-leaf green spinach

NASA Astrophysics Data System (ADS)

Hazarika, S.; Mohanta, D.

2013-01-01

Naturally available green spinach, which is a rich source of potassium, was used as the key ingredient to extract mixed-phase ferroelectric crystals of nitrite and nitrate derivatives (KNO2 + KNO3). The KNO3 phase was found to be dominant for higher pH values, as revealed by the x-ray diffraction patterns. The characteristic optical absorption spectra exhibited intra-band π-π* electronic transitions, whereas Fourier transform infrared spectra exhibited characteristic N-O stretching vibrations. Differential scanning calorimetry revealed a broad endothermic peak at ˜121.8 °C, highlighting a transition from phase II to I via phase III of KNO3. Obtaining nanoscale ferroelectrics via the adoption of green synthesis is economically viable for large-scale production and possible application in ferroelectric elements/devices.

The first report of the physicochemical structure of chitin isolated from Hermetia illucens.

PubMed

Waśko, Adam; Bulak, Piotr; Polak-Berecka, Magdalena; Nowak, Katarzyna; Polakowski, Cezary; Bieganowski, Andrzej

2016-11-01

This is the first report on the physicochemical properties of chitin obtained from larvae and imagoes of black soldier flies (Hermetia illucens). Scanning electron microscopy revealed differences in surface morphologies of the two types of chitin. The crystalline index values of chitins from adult flies and larvae were 24.9% and 35%, respectively. This is a trait that differentiates these biopolymers from chitins extracted from other sources described so far. X-ray diffraction patterns and IR spectroscopy revealed that both types of samples of chitin were in an α crystalline form. Also, the results of elemental analysis, thermal stabilities and FTIR spectroscopy of the chitins from larvae and adults of H. illucens were similar, which points to a general similarity in their physicochemical structure. Copyright © 2016 Elsevier B.V. All rights reserved.

Anomalous Diffraction in Crystallographic Phase Evaluation

PubMed Central

Hendrickson, Wayne A.

2014-01-01

X-ray diffraction patterns from crystals of biological macromolecules contain sufficient information to define atomic structures, but atomic positions are inextricable without having electron-density images. Diffraction measurements provide amplitudes, but the computation of electron density also requires phases for the diffracted waves. The resonance phenomenon known as anomalous scattering offers a powerful solution to this phase problem. Exploiting scattering resonances from diverse elements, the methods of multiwavelength anomalous diffraction (MAD) and single-wavelength anomalous diffraction (SAD) now predominate for de novo determinations of atomic-level biological structures. This review describes the physical underpinnings of anomalous diffraction methods, the evolution of these methods to their current maturity, the elements, procedures and instrumentation used for effective implementation, and the realm of applications. PMID:24726017

Amplitude-phase characteristics of electromagnetic fields diffracted by a hole in a thin film with realistic optical properties

NASA Astrophysics Data System (ADS)

Dorofeyev, Illarion

2009-03-01

Characteristics of a quasi-spherical wave front of an electromagnetic field diffracted by a subwavelength hole in a thin film with real optical properties are studied. Related diffraction problem is solved in general by use of the scalar and vector Green's theorems and related Green's function of a boundary-value problem. Local phase deviations of a diffracted wave front from an ideal spherical front are calculated. Diffracted patterns are calculated for the coherent incident fields in case of holes array in a screen of perfect conductivity.

Broadband diffractive lens or imaging element

DOEpatents

Ceglio, Natale M.; Hawryluk, Andrew M.; London, Richard A.; Seppala, Lynn G.

1993-01-01

A broadband diffractive lens or imaging element produces a sharp focus and/or a high resolution image with broad bandwidth illuminating radiation. The diffractive lens is sectored or segmented into regions, each of which focuses or images a distinct narrowband of radiation but all of which have a common focal length. Alternatively, a serial stack of minus filters, each with a diffraction pattern which focuses or images a distinct narrowband of radiation but all of which have a common focal length, is used. The two approaches can be combined. Multifocal broadband diffractive elements can also be formed. Thin film embodiments are described.

Broadband diffractive lens or imaging element

DOEpatents

Ceglio, N.M.; Hawryluk, A.M.; London, R.A.; Seppala, L.G.

1993-10-26

A broadband diffractive lens or imaging element produces a sharp focus and/or a high resolution image with broad bandwidth illuminating radiation. The diffractive lens is sectored or segmented into regions, each of which focuses or images a distinct narrowband of radiation but all of which have a common focal length. Alternatively, a serial stack of minus filters, each with a diffraction pattern which focuses or images a distinct narrowband of radiation but all of which have a common focal length, is used. The two approaches can be combined. Multifocal broadband diffractive elements can also be formed. Thin film embodiments are described. 21 figures.

PyXRD v0.6.7: a free and open-source program to quantify disordered phyllosilicates using multi-specimen X-ray diffraction profile fitting

NASA Astrophysics Data System (ADS)

Dumon, M.; Van Ranst, E.

2016-01-01

This paper presents a free and open-source program called PyXRD (short for Python X-ray diffraction) to improve the quantification of complex, poly-phasic mixed-layer phyllosilicate assemblages. The validity of the program was checked by comparing its output with Sybilla v2.2.2, which shares the same mathematical formalism. The novelty of this program is the ab initio incorporation of the multi-specimen method, making it possible to share phases and (a selection of) their parameters across multiple specimens. PyXRD thus allows for modelling multiple specimens side by side, and this approach speeds up the manual refinement process significantly. To check the hypothesis that this multi-specimen set-up - as it effectively reduces the number of parameters and increases the number of observations - can also improve automatic parameter refinements, we calculated X-ray diffraction patterns for four theoretical mineral assemblages. These patterns were then used as input for one refinement employing the multi-specimen set-up and one employing the single-pattern set-ups. For all of the assemblages, PyXRD was able to reproduce or approximate the input parameters with the multi-specimen approach. Diverging solutions only occurred in single-pattern set-ups, which do not contain enough information to discern all minerals present (e.g. patterns of heated samples). Assuming a correct qualitative interpretation was made and a single pattern exists in which all phases are sufficiently discernible, the obtained results indicate a good quantification can often be obtained with just that pattern. However, these results from theoretical experiments cannot automatically be extrapolated to all real-life experiments. In any case, PyXRD has proven to be useful when X-ray diffraction patterns are modelled for complex mineral assemblages containing mixed-layer phyllosilicates with a multi-specimen approach.

Microgravity

NASA Image and Video Library

2001-06-06

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

Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

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

McGonegle, David, E-mail: d.mcgonegle1@physics.ox.ac.uk; Wark, Justin S.; Higginbotham, Andrew

2015-08-14

A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as maymore » occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. The simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.« less

Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

DOE PAGES

McGonegle, David; Milathianaki, Despina; Remington, Bruce A.; ...

2015-08-11

A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as maymore » occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. In conclusion, the simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.« less

The slip-and-slide algorithm: a refinement protocol for detector geometry

PubMed Central

Ginn, Helen Mary; Stuart, David Ian

2017-01-01

Geometry correction is traditionally plagued by mis-fitting of correlated parameters, leading to local minima which prevent further improvements. Segmented detectors pose an enhanced risk of mis-fitting: even a minor confusion of detector distance and panel separation can prevent improvement in data quality. The slip-and-slide algorithm breaks down effects of the correlated parameters and their associated target functions in a fundamental shift in the approach to the problem. Parameters are never refined against the components of the data to which they are insensitive, providing a dramatic boost in the exploitation of information from a very small number of diffraction patterns. This algorithm can be applied to exploit the adherence of the spot-finding results prior to indexing to a given lattice using unit-cell dimensions as a restraint. Alternatively, it can be applied to the predicted spot locations and the observed reflection positions after indexing from a smaller number of images. Thus, the indexing rate can be boosted by 5.8% using geometry refinement from only 125 indexed patterns or 500 unindexed patterns. In one example of cypovirus type 17 polyhedrin diffraction at the Linac Coherent Light Source, this geometry refinement reveals a detector tilt of 0.3° (resulting in a maximal Z-axis error of ∼0.5 mm from an average detector distance of ∼90 mm) whilst treating all panels independently. Re-indexing and integrating with updated detector geometry reduces systematic errors providing a boost in anomalous signal of sulfur atoms by 20%. Due to the refinement of decoupled parameters, this geometry method also reaches convergence. PMID:29091058

Speckle in the diffraction patterns of Hendricks-Teller and icosahedral glass models

NASA Technical Reports Server (NTRS)

Garg, Anupam; Levine, Dov

1988-01-01

It is shown that the X-ray diffraction patterns from the Hendricks-Teller model for layered systems and the icosahedral glass models for the icosahedral phases show large fluctuations between nearby scattering wave vectors and from sample to sample, that are quite analogous to laser speckle. The statistics of these fluctuations are studied analytically for the first model and via computer simulations for the second. The observability of these effects is discussed briefly.

Elimination of coherent noise in a coherent light imaging system

NASA Technical Reports Server (NTRS)

Grebowsky, G. J.; Hermann, R. L.; Paull, H. B.; Shulman, A. R.

1970-01-01

Optical imaging systems using coherent light introduce objectionable noise into the output image plane. Dust and bubbles on and in lenses cause most of the noise in the output image. This noise usually appears as bull's-eye diffraction patterns in the image. By rotating the lens about the optical axis these diffraction patterns can be essentially eliminated. The technique does not destroy the spatial coherence of the light and permits spatial filtering of the input plane.

Photoelectron and Auger electron diffraction studies of a sulfur-terminated GaAs(001)-(2×6) surface

NASA Astrophysics Data System (ADS)

Shimoda, M.; Tsukamoto, S.; Koguchi, N.

1998-01-01

Core-level X-ray photoelectron diffraction (XPD) and Auger electron diffraction (AED) have been applied to investigate the sulfur-terminated GaAs(001)-(2×6) surface. No forward scattering peaks were found in the XPD pattern of S 2s emission, indicating that adsorbed S atoms form a single layer on the GaAs substrate. In accordance with the zincblende structure of GaAs, the AED patterns of Ga L 3M 45M 45 and As L 3M 45M 45 emission almost coincide with each other, if one of the emissions is rotated by 90° around the [001] direction. This fact suggests that the diffraction patterns mainly reflect the structure of the bulk GaAs crystal. In order to investigate the surface structure, AED patterns in large polar angles were analyzed with single scattering cluster (SSC) calculations. The best result was obtained with a model cluster where the S-S bond length was set at 0.28 nm, 30% shorter than the corresponding length of the ideal (1×1) structure, and the adsorption height was set at 0.12-0.13 nm, 10% shorter than the ideal interlayer distance of GaAs(001) planes. These values are in good agreement with the results of STM measurements. A modulation of the inter-dimer distance was also found, suggesting the existence of missing dimers.

When holography meets coherent diffraction imaging.

PubMed

Latychevskaia, Tatiana; Longchamp, Jean-Nicolas; Fink, Hans-Werner

2012-12-17

The phase problem is inherent to crystallographic, astronomical and optical imaging where only the intensity of the scattered signal is detected and the phase information is lost and must somehow be recovered to reconstruct the object's structure. Modern imaging techniques at the molecular scale rely on utilizing novel coherent light sources like X-ray free electron lasers for the ultimate goal of visualizing such objects as individual biomolecules rather than crystals. Here, unlike in the case of crystals where structures can be solved by model building and phase refinement, the phase distribution of the wave scattered by an individual molecule must directly be recovered. There are two well-known solutions to the phase problem: holography and coherent diffraction imaging (CDI). Both techniques have their pros and cons. In holography, the reconstruction of the scattered complex-valued object wave is directly provided by a well-defined reference wave that must cover the entire detector area which often is an experimental challenge. CDI provides the highest possible, only wavelength limited, resolution, but the phase recovery is an iterative process which requires some pre-defined information about the object and whose outcome is not always uniquely-defined. Moreover, the diffraction patterns must be recorded under oversampling conditions, a pre-requisite to be able to solve the phase problem. Here, we report how holography and CDI can be merged into one superior technique: holographic coherent diffraction imaging (HCDI). An inline hologram can be recorded by employing a modified CDI experimental scheme. We demonstrate that the amplitude of the Fourier transform of an inline hologram is related to the complex-valued visibility, thus providing information on both, the amplitude and the phase of the scattered wave in the plane of the diffraction pattern. With the phase information available, the condition of oversampling the diffraction patterns can be relaxed, and the phase problem can be solved in a fast and unambiguous manner. We demonstrate the reconstruction of various diffraction patterns of objects recorded with visible light as well as with low-energy electrons. Although we have demonstrated our HCDI method using laser light and low-energy electrons, it can also be applied to any other coherent radiation such as X-rays or high-energy electrons.

Scanning digital lithography providing high speed large area patterning with diffraction limited sub-micron resolution

NASA Astrophysics Data System (ADS)

Wen, Sy-Bor; Bhaskar, Arun; Zhang, Hongjie

2018-07-01

A scanning digital lithography system using computer controlled digital spatial light modulator, spatial filter, infinity correct optical microscope and high precision translation stage is proposed and examined. Through utilizing the spatial filter to limit orders of diffraction modes for light delivered from the spatial light modulator, we are able to achieve diffraction limited deep submicron spatial resolution with the scanning digital lithography system by using standard one inch level optical components with reasonable prices. Raster scanning of this scanning digital lithography system using a high speed high precision x-y translation stage and piezo mount to real time adjust the focal position of objective lens allows us to achieve large area sub-micron resolved patterning with high speed (compared with e-beam lithography). It is determined in this study that to achieve high quality stitching of lithography patterns with raster scanning, a high-resolution rotation stage will be required to ensure the x and y directions of the projected pattern are in the same x and y translation directions of the nanometer precision x-y translation stage.

Direct laser interference patterning of ophthalmic polydimethylsiloxane (PDMS) polymers

NASA Astrophysics Data System (ADS)

Sola, D.; Lavieja, C.; Orera, A.; Clemente, M. J.

2018-07-01

The inscription of diffractive elements in ophthalmic polymers and ocular tissues to induce refractive index changes is of great interest in the fields of Optics and Ophthalmology. In this work fabrication of linear periodic patterns in polydimethylsiloxane (PDMS) intraocular lenses by means of the direct laser interference patterning (DLIP) technique was studied. A Q-Switch Nd:YAG laser coupled to second and third harmonic modules emitting linearly polarized 4 ns pulses at 355 nm with 20 Hz repetition rate was used as the laser source. Laser processing parameters were modified to produce the linear patterns. Processed samples were characterized by means of optical confocal microscopy, Scanning Electron Microscopy SEM, Energy Dispersive X-ray Spectroscopy EDX, Attenuated Total Reflectance-Infrared Spectroscopy ATR-FTIR, and Raman Spectroscopy. Depending on the laser parameters both photo-thermal and photo-chemical damage were observed in the DLIP irradiated areas. Finally, diffractive techniques were used to characterize the diffraction gratings inscribed in the samples resulting in a refractive index change of 1.9 × 10-2 under illumination of a 632.8 nm He-Ne laser.

Diffraction-based overlay metrology for double patterning technologies

NASA Astrophysics Data System (ADS)

Dasari, Prasad; Korlahalli, Rahul; Li, Jie; Smith, Nigel; Kritsun, Oleg; Volkman, Cathy

2009-03-01

The extension of optical lithography to 32nm and beyond is made possible by Double Patterning Techniques (DPT) at critical levels of the process flow. The ease of DPT implementation is hindered by increased significance of critical dimension uniformity and overlay errors. Diffraction-based overlay (DBO) has shown to be an effective metrology solution for accurate determination of the overlay errors associated with double patterning [1, 2] processes. In this paper we will report its use in litho-freeze-litho-etch (LFLE) and spacer double patterning technology (SDPT), which are pitch splitting solutions that reduce the significance of overlay errors. Since the control of overlay between various mask/level combinations is critical for fabrication, precise and accurate assessment of errors by advanced metrology techniques such as spectroscopic diffraction based overlay (DBO) and traditional image-based overlay (IBO) using advanced target designs will be reported. A comparison between DBO, IBO and CD-SEM measurements will be reported. . A discussion of TMU requirements for 32nm technology and TMU performance data of LFLE and SDPT targets by different overlay approaches will be presented.

Effect of cobalt doping on structural and optical properties of nanocrystalline La0.8Pb0.2CrO3 orthochromite

NASA Astrophysics Data System (ADS)

Zarrin, Naima; Shahidhusain

2018-04-01

We have synthesized nanocrystalline La0.8Pb0.2Cr1-xCoxO3 (0≤x≤0.3) through sol-gel process and studied their structural and optical properties. X-ray diffraction patterns reveal that the samples conform in the orthorhombic crystal symmetry with Pnma space group. Structural parameters are refined by Rietveld Refinement using Fullprof software. Lattice parameters and unit cell volume of doped samples are found to decrease with increase in Co doping. The optical energy band gapdecreases whereas Urbach energy increases with the increase in Co content.

Synthesis, structural and optical properties of silver nanoparticles uniformly decorated ZnO nanowires

NASA Astrophysics Data System (ADS)

Zhang, Ke-Xin; Wen, Xing; Yao, Cheng-Bao; Li, Jin; Zhang, Meng; Li, Qiang-Hua; Sun, Wen-Jun; Wu, Jia-Da

2018-04-01

Silver (Ag) nanoparticles decorated Zinc oxide (A-ZnO) nanowires have been successfully synthesized by two-step chemical vapour deposition and magnetron sputtering method. The X-ray diffraction patterns revealed their hexagonal wurtzite structure. SEM images indicated the Ag nanoparticles are distributed uniformly on the surface of A-ZnO nanowires. By extending the sputtering time, the atomic percent of Ag increased gradually. Moreover, the photoluminescence results demonstrated two major emission peaks for the A-ZnO nanowires. Where, the visible emission peaks were stronger than those of unmodified ZnO nanowires. These studies promise their potential applications in multifunctional optical devices.

Room Temperature Magnetic Behavior In Nanocrystalline Ni-Doped Zro2 By Microwave-Assisted Polyol Synthesis

NASA Astrophysics Data System (ADS)

Parimita Rath, Pragyan; Parhi, Pankaj Kumar; Ranjan Panda, Sirish; Priyadarshini, Barsharani; Ranjan Sahoo, Tapas

2017-08-01

This article, deals with a microwave-assisted polyol method to demonstrate a low temperature route < 250°C, to prepare a high temperature cubic zirconia phase. Powder XRD pattern shows broad diffraction peaks suggesting nanometric size of the particles. Magnetic behavior of 1-5 at% Ni doped samples show a threshold for substitutional induced room temperature ferromagnetism up to 3 at% of Ni. TGA data reveals that Ni-doped ZrO2 polyol precursors decompose exothermically below 300°C. IR data confirms the reduction of Zr(OH)4 precipitates to ZrO2, in agreement with the conclusions drawn from the TGA analysis.

Structural, electronic transport and optical properties of Cr doped PbS thin film by chemical bath deposition

NASA Astrophysics Data System (ADS)

Preetha, K. C.

2017-06-01

Incorporation of Chromium ions into Lead Sulphide thin films have been achieved by CBD technique. Effects of doping were investigated as a function of Pb/Cr ratio from o to 2 at %. X-ray diffraction patterns showed that films were polycrystalline in nature with increase in crystallite size up to an optimum doping concentration. Scanning electron microscopic study revealed excellent morphology with doping concentration. The low transmittance in the UV-VIS region offered the suitability of the samples as solar control coatings. The thin films were found to be P type and electrical conductivity enhanced on doping.

Observation of ferromagnetism in Mn doped KNbO3

NASA Astrophysics Data System (ADS)

Manikandan, M.; Venkateswaran, C.

2015-06-01

Pure and Mn doped KNbO3 have been prepared by ball milling assisted ceramic method. Mn ion had been doped at Nb site to induce ferromagnetism at room temperature. X-ray diffraction (XRD) patterns reveal the formation of orthorhombic phase. High resolution scanning electron micrograph (HR-SEM) of both pure and Mn doped samples show a mixture of spherical and plate like particles. Room temperature magnetic behavior of both the samples were analyzed using vibrating sample magnetometer (VSM). 5% Mn doped KNbO3 exhibits ferromagnetic behavior. Observed ferromagnetic feature has been explained by interactions between bound magnetic polarons which are created by Mn4+ ions.

Metallocarbohedrenes: Transmission Electron Microscopy of Mass Gated Deposits

NASA Astrophysics Data System (ADS)

Castleman, M. E. Lyn, Jr.

2002-03-01

Titanium and zirconium Met-Car cluster ions have been detected from the direct laser vaporization of metal-graphite mixtures using time-of-flight mass spectrometry. Optimization of the production conditions enabled sufficient intensities to mass select and deposit Met-Cars on surfaces. High-resolution transmission electron microscopy images of mass gated Met-Car species reveals deposited nanocrystals 2 nm in diameter. Diffraction patterns indicate the presence of multiple species and shows that the deposits have spatial orientation. Lattice parameters have been extracted. The implication of the findings will be discussed. Support for the work has been from the AFOSR F49620-01-1-0122.

Electrode-stress-induced nanoscale disorder in Si quantum electronic devices

DOE PAGES

Park, J.; Ahn, Y.; Tilka, J. A.; ...

2016-06-20

Disorder in the potential-energy landscape presents a major obstacle to the more rapid development of semiconductor quantum device technologies. We report a large-magnitude source of disorder, beyond commonly considered unintentional background doping or fixed charge in oxide layers: nanoscale strain fields induced by residual stresses in nanopatterned metal gates. Quantitative analysis of synchrotron coherent hard x-ray nanobeam diffraction patterns reveals gate-induced curvature and strains up to 0.03% in a buried Si quantum well within a Si/SiGe heterostructure. Furthermore, electrode stress presents both challenges to the design of devices and opportunities associated with the lateral manipulation of electronic energy levels.

Chemistry Notes

ERIC Educational Resources Information Center

School Science Review, 1972

1972-01-01

Short articles describe preparation of clean iron sheet for corrosion experiments, models of crystalline structures using glass marbles, photographic production of diffraction grids for producing analogies of X-ray diffraction patterns, and a simple method of determining a reactivity series for the common metals. (AL)

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

NASA Technical Reports Server (NTRS)

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

X-ray diffraction patterns and diffracted intensity of Kα spectral lines of He-like ions

NASA Astrophysics Data System (ADS)

Goyal, Arun; Khatri, Indu; Singh, A. K.; Sharma, Rinku; Mohan, Man

2017-09-01

In the present paper, we have calculated fine-structure energy levels related to the configurations 1s2s, 1s2p, 1s3s and 1s3p by employing GRASP2K code. We have also computed radiative data for transitions from 1s2p 1 P1o, 1s2p 3 P2o, 1s2p 3 P1o and 1s2s 3S1 to the ground state 1s2. We have made comparisons of our presented energy levels and transition wavelengths with available results compiled by NIST and good agreement is achieved. We have also provided X-ray diffraction (XRD) patterns of Kα spectral lines, namely w, x, y and z of Cu XXVIII, Kr XXXV and Mo with diffraction angle and maximum diffracted intensity which is not published elsewhere in the literature. We believe that our presented results may be beneficial in determination of the order parameter, X-ray crystallography, solid-state drug analysis, forensic science, geological and medical applications.

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

Low-kilovolt coherent electron diffractive imaging instrument based on a single-atom electron source

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

Lin, Chun-Yueh; Chang, Wei-Tse; Chen, Yi-Sheng

2016-03-15

In this work, a transmission-type, low-kilovolt coherent electron diffractive imaging instrument was constructed. It comprised a single-atom field emitter, a triple-element electrostatic lens, a sample holder, and a retractable delay line detector to record the diffraction patterns at different positions behind the sample. It was designed to image materials thinner than 3 nm. The authors analyzed the asymmetric triple-element electrostatic lens for focusing the electron beams and achieved a focused beam spot of 87 nm on the sample plane at the electron energy of 2 kV. High-angle coherent diffraction patterns of a suspended graphene sample corresponding to (0.62 Å){sup −1} were recorded. This workmore » demonstrated the potential of coherent diffractive imaging of thin two-dimensional materials, biological molecules, and nano-objects at a voltage between 1 and 10 kV. The ultimate goal of this instrument is to achieve atomic resolution of these materials with high contrast and little radiation damage.« less

X-ray diffraction study of nanocrystalline and amorphous structure within major and minor ampullate dragline spider silks

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

Sampath, Sujatha; Isdebski, Thomas; Jenkins, Janelle E.

Synchrotron X-ray micro-diffraction experiments were carried out on Nephila clavipes (NC) and Argiope aurantia (AA) major (MA) and minor ampullate (MiA) fibers that make up dragline spider silk. The diffraction patterns show a semi-crystalline structure with {beta}-poly(L-alanine) nanocrystallites embedded in a partially oriented amorphous matrix. A superlattice reflection 'S' diffraction ring is observed, which corresponds to a crystalline component larger in size and is poorly oriented, when compared to the {beta}-poly(L-alanine) nanocrystallites that are commonly observed in dragline spider silks. Crystallite size, crystallinity and orientation about the fiber axis have been determined from the wide-angle X-ray diffraction (WAXD) patterns. Inmore » both NC and AA, the MiA silks are found to be more highly crystalline, when compared with the corresponding MA silks. Detailed analysis on the amorphous matrix shows considerable differences in the degree of order of the oriented amorphous component between the different silks studied and may play a crucial role in determining the mechanical properties of the silks.« less

Green synthesis of gold nanoparticles using Citrus fruits (Citrus limon, Citrus reticulata and Citrus sinensis) aqueous extract and its characterization.

PubMed

Sujitha, Mohanan V; Kannan, Soundarapandian

2013-02-01

This study reports the biological synthesis of gold nanoparticles by the reduction of HAuCl(4) by using citrus fruits (Citrus limon, Citrus reticulata and Citrus sinensis) juice extract as the reducing and stabilizing agent. A various shape and size of gold nanoparticles were formed when the ratio of the reactants were altered with respect to 1.0mM chloroauric acid solution. The gold nanoparticles obtained were characterized by UV-visible spectra, transmission electron microscopy (TEM) and X-ray diffraction (XRD). TEM studies showed the particles to be of various shapes and sizes and particle size ranges from 15 to 80 nm. Selected-area electron diffraction (SAED) pattern confirmed fcc phase and crystallinity of the particles. The X-ray diffraction analysis revealed the distinctive facets (111, 200, 220 and 222 planes) of gold nanoparticles. Dynamic light scattering (DLS) studies revealed that the average size for colloid gp(3) of C. limon, C. reticulata and C. sinensis are 32.2 nm, 43.4 nm and 56.7 nm respectively. The DLS graph showed that the particles size was larger and more polydispersed compared to the one observed by TEM due to the fact that the measured size also includes the bio-organic compounds enveloping the core of the Au NPs. Zeta potential value for gold nanoparticles obtained from colloid gp(3) of C. limon, C. reticulata and C. sinensis are -45.9, -37.9 and -31.4 respectively indicating the stability of the synthesized nanoparticles. Herein we propose a novel, previously unexploited method for the biological syntheses of polymorphic gold nanoparticles with potent biological applications. Copyright © 2012 Elsevier B.V. All rights reserved.

High-resolution synchrotron x-ray powder diffraction study of the incommensurate modulation in the martensite phase of Ni2MnGa: Evidence for nearly 7M modulation and phason broadening

NASA Astrophysics Data System (ADS)

Singh, Sanjay; Petricek, V.; Rajput, Parasmani; Hill, Adrian H.; Suard, E.; Barman, S. R.; Pandey, Dhananjai

2014-07-01

The modulated structure of the martensite phase of Ni2MnGa is revisited using high-resolution synchrotron x-ray powder diffraction measurements, which reveal higher-order satellite reflections up to the third order and phason broadening of the satellite peaks. The structure refinement, using the (3+1) dimensional superspace group approach, shows that the modulated structure of Ni2MnGa can be described by orthorhombic superspace group Immm(00γ)s00 with lattice parameters a=4.218 61(2)Å,b=5.546 96(3)Å, and c=4.187 63(2) Å, and an incommensurate modulation wave vector q =0.43160(3)c*=(3/7+δ)c*, where δ =0.00303(3) is the degree of incommensuration of the modulated structure. Additional satellite peak broadening, which could not be accounted for in terms of the anisotropic strain broadening based on a lattice parameter distribution, has been modeled in terms of phasons using fourth-rank covariant strain-tensor representation for incommensurate structures. The simulation of single-crystal diffraction patterns from the refined structural parameters unambiguously reveals a rational approximant structure with 7M modulation. The inhomogeneous displacement of different atomic sites on account of incommensurate modulation and the presence of phason broadening clearly rule out the adaptive phase model proposed recently by Kaufmann et al. [S. Kaufmann, U. K. Rößler, O. Heczko, M. Wuttig, J. Buschbeck, L. Schultz, and S. Fähler, Phys. Rev. Lett. 104, 145702 (2010), 10.1103/PhysRevLett.104.145702] and suggest that the modulation in Ni2MnGa originates from soft-mode phonons.

CD, DVD, and Blu-Ray Disc Diffraction with a Laser Ray Box

ERIC Educational Resources Information Center

DeWeerd, Alan J.

2016-01-01

A compact disc (CD) can be used as a diffraction grating, even though its track consists of a series of pits, not a continuous groove. Previous authors described how to measure the track spacing on a CD using an incident laser beam normal to the surface or one at an oblique angle. In both cases, the diffraction pattern was projected on a screen…

JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

Treesearch

Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

2006-01-01

X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

Transmission X-ray Diffraction (XRD) Patterns Relevant to the MSL Chemin Amorphous Component: Sulfates And Silicates

NASA Technical Reports Server (NTRS)

Morris, R. V.; Rampe, E. B.; Graff, T. G.; Archer, P. D., Jr.; Le, L.; Ming, D. W.; Sutter, B.

2015-01-01

The Mars Science Laboratory (MSL) CheMin instrument on the Curiosity rover is a transmission X-ray diffractometer (Co-Kalpha radiation source and a approx.5deg to approx.52deg 2theta range) where the analyzed powder samples are constrained to have discrete particle diameters <150 microns by a sieve. To date, diffraction patterns have been obtained for one basaltic soil (Rocknest (RN)) and four drill fines of coherent rock (John Klein (JK), Cumberland (CB), Windjana (WJ), and Confidence Hills (CH)). The CheMin instrument has detected and quantified the abundance of both primary igneous (e.g., feldspar, olivine, and pyroxene) and secondary (e.g., Ca-sulfates, hematite, akaganeite, and Fe-saponite) minerals. The diffraction patterns of all CheMin samples are also characterized by a broad diffraction band centered near 30deg 2theta and by increasing diffraction intensity (scattering continuum) from approx.15deg to approx.5deg, the 2theta minimum. Both the broad band and the scattering continuum are attributed to the presence of an XRD amorphous component. Estimates of amorphous component abundance, based on the XRD data itself and on mass-balance calculations using APXS data crystalline component chemistry derived from XRD data, martian meteorites, and/or stoichiometry [e.g., 6-9], range from approx.20 wt.% to approx.50 wt.% of bulk sample. The APXSbased calculations show that the amorphous component is rich in volatile elements (esp. SO3) and is not simply primary basaltic glass, which was used as a surrogate to model the broad band in the RN CheMin pattern. For RN, the entire volatile inventory (except minor anhydrite) is assigned to the amorphous component because no volatile-bearing crystalline phases were reported within detection limits [2]. For JK and CB, Fesaponite, basanite, and akaganeite are volatile-bearing crystalline components. Here we report transmission XRD patterns for sulfate and silicate phases relevant to interpretation of MSL-CheMin XRD amorphous components.

Digital direct electron imaging of energy-filtered electron backscatter diffraction patterns

NASA Astrophysics Data System (ADS)

Vespucci, S.; Winkelmann, A.; Naresh-Kumar, G.; Mingard, K. P.; Maneuski, D.; Edwards, P. R.; Day, A. P.; O'Shea, V.; Trager-Cowan, C.

2015-11-01

Electron backscatter diffraction is a scanning electron microscopy technique used to obtain crystallographic information on materials. It allows the nondestructive mapping of crystal structure, texture, and strain with a lateral and depth resolution on the order of tens of nanometers. Electron backscatter diffraction patterns (EBSPs) are presently acquired using a detector comprising a scintillator coupled to a digital camera, and the crystallographic information obtainable is limited by the conversion of electrons to photons and then back to electrons again. In this article we will report the direct acquisition of energy-filtered EBSPs using a digital complementary metal-oxide-semiconductor hybrid pixel detector, Timepix. We show results from a range of samples with different mass and density, namely diamond, silicon, and GaN. Direct electron detection allows the acquisition of EBSPs at lower (≤5 keV) electron beam energies. This results in a reduction in the depth and lateral extension of the volume of the specimen contributing to the pattern and will lead to a significant improvement in lateral and depth resolution. Direct electron detection together with energy filtering (electrons having energy below a specific value are excluded) also leads to an improvement in spatial resolution but in addition provides an unprecedented increase in the detail in the acquired EBSPs. An increase in contrast and higher-order diffraction features are observed. In addition, excess-deficiency effects appear to be suppressed on energy filtering. This allows the fundamental physics of pattern formation to be interrogated and will enable a step change in the use of electron backscatter diffraction (EBSD) for crystal phase identification and the mapping of strain. The enhancement in the contrast in high-pass energy-filtered EBSD patterns is found to be stronger for lighter, less dense materials. The improved contrast for such materials will enable the application of the EBSD technique to be expanded to materials for which conventional EBSD analysis is not presently practicable.

Room temperature chemical bath deposition of cadmium selenide, cadmium sulfide and cadmium sulfoselenide thin films with novel nanostructures

NASA Astrophysics Data System (ADS)

VanderHyde, Cephas A.; Sartale, S. D.; Patil, Jayant M.; Ghoderao, Karuna P.; Sawant, Jitendra P.; Kale, Rohidas B.

2015-10-01

A simple, convenient and low cost chemical synthesis route has been used to deposit nanostructured cadmium sulfide, selenide and sulfoselenide thin films at room temperature. The films were deposited on glass substrates, using cadmium acetate as cadmium ion and sodium selenosulfate/thiourea as a selenium/sulfur ion sources. Aqueous ammonia was used as a complex reagent and also to adjust the pH of the final solution. The as-deposited films were uniform, well adherent to the glass substrate, specularly reflective and red/yellow in color depending on selenium and sulfur composition. The X-ray diffraction pattern of deposited cadmium selenide thin film revealed the nanocrystalline nature with cubic phase; cadmium sulfide revealed mixture of cubic along with hexagonal phase and cadmium sulfoselenide thin film were grown with purely hexagonal phase. The morphological observations revealed the growth and formation of interesting one, two and three-dimensional nanostructures. The band gap of thin films was calculated and the results are reported.

Investigation of Embedded Si/C System Exposed to a Hybrid Reaction of Centrifugal-Assisted Thermite Method

PubMed Central

Mahmoodian, Reza; Yahya, Rosiyah; Dabbagh, Ali; Hamdi, Mohd; Hassan, Mohsen A.

2015-01-01

A novel method is proposed to study the behavior and phase formation of a Si+C compacted pellet under centrifugal acceleration in a hybrid reaction. Si+C as elemental mixture in the form of a pellet is embedded in a centrifugal tube. The pellet assembly and tube are exposed to the sudden thermal energy of a thermite reaction resulted in a hybrid reaction. The hybrid reaction of thermite and Si+C produced unique phases. X-ray diffraction pattern (XRD) as well as microstructural and elemental analyses are then investigated. XRD pattern showed formation of materials with possible electronic and magnetic properties. The cooling rate and the molten particle viscosity mathematical model of the process are meant to assist in understanding the physical and chemical phenomena took place during and after reaction. The results analysis revealed that up to 85% of materials converted into secondary products as ceramics-matrix composite. PMID:26641651

Investigation of Embedded Si/C System Exposed to a Hybrid Reaction of Centrifugal-Assisted Thermite Method.

PubMed

Mahmoodian, Reza; Yahya, Rosiyah; Dabbagh, Ali; Hamdi, Mohd; Hassan, Mohsen A

2015-01-01

A novel method is proposed to study the behavior and phase formation of a Si+C compacted pellet under centrifugal acceleration in a hybrid reaction. Si+C as elemental mixture in the form of a pellet is embedded in a centrifugal tube. The pellet assembly and tube are exposed to the sudden thermal energy of a thermite reaction resulted in a hybrid reaction. The hybrid reaction of thermite and Si+C produced unique phases. X-ray diffraction pattern (XRD) as well as microstructural and elemental analyses are then investigated. XRD pattern showed formation of materials with possible electronic and magnetic properties. The cooling rate and the molten particle viscosity mathematical model of the process are meant to assist in understanding the physical and chemical phenomena took place during and after reaction. The results analysis revealed that up to 85% of materials converted into secondary products as ceramics-matrix composite.

Comments on ”Evidence of the hydrogen release mechanism in bulk MgH2”

NASA Astrophysics Data System (ADS)

Surrey, Alexander; Nielsch, Kornelius; Rellinghaus, Bernd

2017-04-01

The effect of an electron beam induced dehydrogenation of MgH2 in the transmission electron microscope (TEM) is largely underestimated by Nogita et al., and led the authors to a misinterpretation of their TEM observations. Firstly, the selected area diffraction (SAD) pattern is falsely interpreted. A re-evaluation of the SAD pattern reveals that no MgH2 is present in the sample, but that it rather consists of Mg and MgO only. Secondly, the transformation of the sample upon in-situ heating in the TEM cannot be ascribed to dehydrogenation, but is rather to be explained by the (nanoscale) Kirkendall effect, which leads to the formation of hollow MgO shells without any metallic Mg in their cores. Hence, the conclusions drawn from the TEM investigation are invalid, as the authors apparently have never studied MgH2.

Final Technical Report: Application of in situ Neutron Diffraction to Understand the Mechanism of Phase Transitions

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

Chandran, Ravi

In this research, phase transitions in the bulk electrodes for Li-ion batteries were investigated using neutron diffraction (ND) as well as neutron imaging techniques. The objectives of this research is to design of a novel in situ electrochemical cell to obtain Rietveld refinable neutron diffraction experiments using small volume electrodes of various laboratory/research-scale electrodes intended for Li-ion batteries. This cell is also to be used to investigate the complexity of phase transitions in Li(Mg) alloy electrodes, either by diffraction or by neutron imaging, which occur under electrochemical lithiation and delithiation, and to determine aspects of phase transition that enable/limit energymore » storage capacity. Additional objective is to investigate the phase transitions in electrodes made of etched micro-columns of silicon and investigate the effect of particle/column size on phase transitions and nonequilibrium structures. An in situ electrochemical cell was designed successfully and was used to study the phase transitions under in-situ neutron diffraction in both the electrodes (anode/cathode) simultaneously in graphite/LiCoO 2 and in graphite/LiMn 2O 4 cells each with two cells. The diffraction patterns fully validated the working of the in situ cell. Additional experimental were performed using the Si micro-columnar electrodes. The results revealed new lithiation phenomena, as evidenced by mosaicity formation in silicon electrode. These experiments were performed in Vulcan diffractometer at SNS, Oak Ridge National Laboratory. In parallel, the spatial distribution of Li during lithiation and delithiation processes in Li-battery electrodes were investigated. For this purpose, neutron tomographic imaging technique has been used for 3D mapping of Li distribution in bulk Li(Mg) alloy electrodes. It was possible to observe the phase boundary of Li(Mg) alloy indicating phase transition from Li-rich BCC β-phase to Li-lean α-phase. These experiments have been performed at CG-1D Neutron Imaging Prototype Station at SNS.« less

X-ray absorption microtomography (microCT) and small beam diffraction mapping of sea urchin teeth.

PubMed

Stock, S R; Barss, J; Dahl, T; Veis, A; Almer, J D

2002-07-01

Two noninvasive X-ray techniques, laboratory X-ray absorption microtomography (microCT) and X-ray diffraction mapping, were used to study teeth of the sea urchin Lytechinus variegatus. MicroCT revealed low attenuation regions at near the tooth's stone part and along the carinar process-central prism boundary; this latter observation appears to be novel. The expected variation of Mg fraction x in the mineral phase (calcite, Ca(1-x)Mg(x)CO(3)) cannot account for all of the linear attenuation coefficient decrease in the two zones: this suggested that soft tissue is localized there. Transmission diffraction mapping (synchrotron X-radiation, 80.8 keV, 0.1 x 0.1mm(2) beam area, 0.1mm translation grid, image plate area detector) simultaneously probed variations in 3-D and showed that the crystal elements of the "T"-shaped tooth were very highly aligned. Diffraction patterns from the keel (adaxial web) and from the abaxial flange (containing primary plates and the stone part) differed markedly. The flange contained two populations of identically oriented crystal elements with lattice parameters corresponding to x=0.13 and x=0.32. The keel produced one set of diffraction spots corresponding to the lower x. The compositions were more or less equivalent to those determined by others for camarodont teeth, and the high Mg phase is expected to be disks of secondary mineral epitaxially related to the underlying primary mineral element. Lattice parameter gradients were not noted in the keel or flange. Taken together, the microCT and diffraction results indicated that there was a band of relatively high protein content, of up to approximately 0.25 volume fraction, in the central part of the flange and paralleling its adaxial and abaxial faces. X-ray microCT and microdiffraction data used in conjunction with protein distribution data will be crucial for understanding the properties of various biocomposites and their mechanical functions.

Myosin Heads Are Displaced from Actin Filaments in the In Situ Beating Rat Heart in Early Diabetes

PubMed Central

Jenkins, Mathew J.; Pearson, James T.; Schwenke, Daryl O.; Edgley, Amanda J.; Sonobe, Takashi; Fujii, Yutaka; Ishibashi-Ueda, Hatsue; Kelly, Darren J.; Yagi, Naoto; Shirai, Mikiyasu

2013-01-01

Diabetes is independently associated with a specific cardiomyopathy, characterized by impaired cardiac muscle relaxation and force development. Using synchrotron radiation small-angle x-ray scattering, this study investigated in the in situ heart and in real-time whether changes in cross-bridge disposition and myosin interfilament spacing underlie the early development of diabetic cardiomyopathy. Experiments were conducted using anesthetized Sprague-Dawley rats 3 weeks after treatment with either vehicle (control) or streptozotocin (diabetic). Diffraction patterns were recorded during baseline and dobutamine infusions simultaneous with ventricular pressure-volumetry. From these diffraction patterns myosin mass transfer to actin filaments was assessed as the change in intensity ratio (I1,0/I1,1). In diabetic hearts cross-bridge disposition was most notably abnormal in the diastolic phase (p < 0.05) and to a lesser extent the systolic phase (p < 0.05). In diabetic rats only, there was a transmural gradient of contractile depression. Elevated diabetic end-diastolic intensity ratios were correlated with the suppression of diastolic function (p < 0.05). Furthermore, the expected increase in myosin head transfer by dobutamine was significantly blunted in diabetic animals (p < 0.05). Interfilament spacing did not differ between groups. We reveal that impaired cross-bridge disposition and radial transfer may thus underlie the early decline in ventricular function observed in diabetic cardiomyopathy. PMID:23473489

Energy-selective Neutron Imaging for Three-dimensional Non-destructive Probing of Crystalline Structures

NASA Astrophysics Data System (ADS)

Peetermans, S.; Bopp, M.; Vontobel, P.; Lehmann, E. H.

Common neutron imaging uses the full polychromatic neutron beam spectrum to reveal the material distribution in a non-destructive way. Performing it with a reduced energy band, i.e. energy-selective neutron imaging, allows access to local variation in sample crystallographic properties. Two sample categories can be discerned with different energy responses. Polycrystalline materials have an energy-dependent cross-section featuring Bragg edges. Energy-selective neutron imaging can be used to distinguish be- tween crystallographic phases, increase material sensitivity or penetration, improve quantification etc. An example of the latter is shown by the examination of copper discs prior to machining them into linear accelerator cavity structures. The cross-section of single crystals features distinct Bragg peaks. Based on their pattern, one can determine the orientation of the crystal, as in a Laue pattern, but with the tremendous advantage that the operation can be performed for each pixel, yielding crystal orientation maps at high spatial resolution. A wholly different method to investigate such samples is also introduced: neutron diffraction imaging. It is based on projections formed by neutrons diffracted from the crystal lattice out of the direct beam. The position of these projections on the detector gives information on the crystal orientation. The projection itself can be used to reconstruct the crystal shape. A three-dimensional mapping of local Bragg reflectivity or a grain orientation mapping can thus be obtained.

DIFFRACTION FROM MODEL CRYSTALS

USDA-ARS?s Scientific Manuscript database

Although calculating X-ray diffraction patterns from atomic coordinates of a crystal structure is a widely available capability, calculation from non-periodic arrays of atoms has not been widely applied to cellulose. Non-periodic arrays result from modeling studies that, even though started with at...

Subreflector extension for improved efficiencies in Cassegrain antennas - GTD/PO analysis. [Geometrical Theory of Diffraction/Physical Optics

NASA Technical Reports Server (NTRS)

Rahmat-Samii, Yahya

1986-01-01

Both offset and symmetric Cassegrain reflector antennas are used in satellite and ground communication systems. It is known that the subreflector diffraction can degrade the performance of these reflectors. A geometrical theory of diffraction/physical optics analysis technique is used to investigate the effects of the extended subreflector, beyond its optical rim, on the reflector efficiency and far-field patterns. Representative numerical results are shown for an offset Cassegrain reflector antenna with different feed illumination tapers and subreflector extensions. It is observed that for subreflector extensions as small as one wavelength, noticeable improvements in the overall efficiencies can be expected. Useful design data are generated for the efficiency curves and far-field patterns.

Replication of Holograms with Corn Syrup by Rubbing

PubMed Central

Mejias-Brizuela, Nildia Y.; Olivares-Pérez, Arturo; Ortiz-Gutiérrez, Mauricio

2012-01-01

Corn syrup films are used to replicate holograms in order to fabricate micro-structural patterns without the toxins commonly found in photosensitive salts and dyes. We use amplitude and relief masks with lithographic techniques and rubbing techniques in order to transfer holographic information to corn syrup material. Holographic diffraction patterns from holographic gratings and computer Fourier holograms fabricated with corn syrup are shown. We measured the diffraction efficiency parameter in order to characterize the film. The versatility of this material for storage information is promising. Holographic gratings achieved a diffraction efficiency of around 8.4% with an amplitude mask and 36% for a relief mask technique. Preliminary results using corn syrup as an emulsion for replicating holograms are also shown in this work.

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.

"XANSONS for COD": a new small BOINC project in crystallography

NASA Astrophysics Data System (ADS)

Neverov, Vladislav S.; Khrapov, Nikolay P.

2018-04-01

"XANSONS for COD" (http://xansons4cod.com) is a new BOINC project aimed at creating the open-access database of simulated x-ray and neutron powder diffraction patterns for nanocrystalline phase of materials from the collection of the Crystallography Open Database (COD). The project uses original open-source software XaNSoNS to simulate diffraction patterns on CPU and GPU. This paper describes the scientific problem this project solves, the project's internal structure, its operation principles and organization of the final database.

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.

Interpretation of small-angle diffraction experiments on opal-like photonic crystals

NASA Astrophysics Data System (ADS)

Marlow, F.; Muldarisnur, M.; Sharifi, P.; Zabel, H.

2011-08-01

Comprehensive structural information on artificial opals involving the deviations from the strongly dominating face-centered cubic structure is still missing. Recent structure investigations with neutrons and synchrotron sources have shown a high degree of order but also a number of unexpected scattering features. Here, we point out that the exclusion of the allowed 002-type diffraction peaks by a small atomic form factor is not obvious and that surface scattering has to be included as a possible source for the diffraction peaks. Our neutron diffraction data indicate that surface scattering is the main reason for the smallest-angle peaks in the diffraction patterns.

Ultrafast electron diffraction with megahertz MeV electron pulses from a superconducting radio-frequency photoinjector

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

Feng, L. W.; Lin, L.; Huang, S. L.

We report ultrafast relativistic electron diffraction operating at the megahertz repetition rate where the electron beam is produced in a superconducting radio-frequency (rf) photoinjector. We show that the beam quality is sufficiently high to provide clear diffraction patterns from gold and aluminium samples. With the number of electrons, several orders of magnitude higher than that from a normal conducting photocathode rf gun, such high repetition rate ultrafast MeV electron diffraction may open up many new opportunities in ultrafast science.

Increased understanding of cellulose crystallinity

USDA-ARS?s Scientific Manuscript database

According to the International Union of Crystallography, “material is a crystal if it has essentially a sharp diffraction pattern. The word essentially means that most of the intensity of the diffraction is concentrated in relatively sharp Bragg peaks, besides the always present diffuse scattering.”...

Diffraction Plates for Classroom Demonstrations

ERIC Educational Resources Information Center

Hoover, Richard B.

1969-01-01

Describes the computer generation of random and regular arrays of apertures on photographic film and their applications for classroom demonstrations of the Fraunhofer patterns produced by simple and complex apertures, Babinet's principle, resolution according to the Rayleigh criterion, and many other aspects of diffraction. (LC)

Idealized powder diffraction patterns for cellulose polymorphs

USDA-ARS?s Scientific Manuscript database

Cellulose samples are routinely analyzed by X-ray diffraction to determine their crystal type (polymorph) and crystallinity. However, the connection is seldom made between those efforts and the crystal structures of cellulose that have been determined with synchrotron X-radiation and neutron diffrac...

Near-field limitations of Fresnel-regime coherent diffraction imaging

DOE PAGES

Pound, Benjamin A.; Barber, John L.; Nguyen, Kimberly; ...

2017-08-04

Coherent diffraction imaging (CDI) is a rapidly developing form of imaging that offers the potential of wavelength-limited resolution without image-forming lenses. In CDI, the intensity of the diffraction pattern is measured directly by the detector, and various iterative phase retrieval algorithms are used to “invert” the diffraction pattern and reconstruct a high-resolution image of the sample. But, there are certain requirements in CDI that must be met to reconstruct the object. Although most experiments are conducted in the “far-field”—or Fraunhofer—regime where the requirements are not as stringent, some experiments must be conducted in the “near field” where Fresnel diffraction mustmore » be considered. According to the derivation of Fresnel diffraction, successful reconstructions can only be obtained when the small-angle number, a derived quantity, is much less than one. We show, however, that it is not actually necessary to fulfill the small-angle condition. The Fresnel kernel well approximates the exact kernel in regions where the phase oscillates slowly, and in regions of fast oscillations, indicated by large A n , the error between kernels should be negligible due to stationary-phase arguments. Finally we verify, by experiment, this conclusion with a helium neon laser setup and show that it should hold at x-ray wavelengths as well.« less

Quasi-parallel precession diffraction: Alignment method for scanning transmission electron microscopes.

PubMed

Plana-Ruiz, S; Portillo, J; Estradé, S; Peiró, F; Kolb, Ute; Nicolopoulos, S

2018-06-06

A general method to set illuminating conditions for selectable beam convergence and probe size is presented in this work for Transmission Electron Microscopes (TEM) fitted with µs/pixel fast beam scanning control, (S)TEM, and an annular dark field detector. The case of interest of beam convergence and probe size, which enables diffraction pattern indexation, is then used as a starting point in this work to add 100 Hz precession to the beam while imaging the specimen at a fast rate and keeping the projector system in diffraction mode. The described systematic alignment method for the adjustment of beam precession on the specimen plane while scanning at fast rates is mainly based on the sharpness of the precessed STEM image. The complete alignment method for parallel condition and precession, Quasi-Parallel PED-STEM, is presented in block diagram scheme, as it has been tested on a variety of instruments. The immediate application of this methodology is that it renders the TEM column ready for the acquisition of Precessed Electron Diffraction Tomographies (EDT) as well as for the acquisition of slow Precessed Scanning Nanometer Electron Diffraction (SNED). Examples of the quality of the Precessed Electron Diffraction (PED) patterns and PED-STEM alignment images are presented with corresponding probe sizes and convergence angles. Copyright © 2018. Published by Elsevier B.V.

New in-situ neutron diffraction cell for electrode materials

NASA Astrophysics Data System (ADS)

Biendicho, Jordi Jacas; Roberts, Matthew; Offer, Colin; Noréus, Dag; Widenkvist, Erika; Smith, Ronald I.; Svensson, Gunnar; Edström, Kristina; Norberg, Stefan T.; Eriksson, Sten G.; Hull, Stephen

2014-02-01

A novel neutron diffraction cell has been constructed to allow in-situ studies of the structural changes in materials of relevance to battery applications during charge/discharge cycling. The new design is based on the coin cell geometry, but has larger dimensions compared to typical commercial batteries in order to maximize the amount of electrode material and thus, collect diffraction data of good statistical quality within the shortest possible time. An important aspect of the design is its modular nature, allowing flexibility in both the materials studied and the battery configuration. This paper reports electrochemical tests using a Nickel-metal-hydride battery (Ni-MH), which show that the cell is able to deliver 90% of its theoretical capacity when using deuterated components. Neutron diffraction studies performed on the Polaris diffractometer using nickel metal and a hydrogen-absorbing alloy (MH) clearly show observable changes in the neutron diffraction patterns as a function of the discharge state. Due to the high quality of the diffraction patterns collected in-situ (i.e. good peak-to-background ratio), phase analysis and peak indexing can be performed successfully using data collected in around 30 min. In addition to this, structural parameters for the β-phase (charged) MH electrode obtained by Rietveld refinement are presented.

Near-field limitations of Fresnel-regime coherent diffraction imaging

NASA Astrophysics Data System (ADS)

Pound, Benjamin A.; Barber, John L.; Nguyen, Kimberly; Tyson, Matthew C.; Sandberg, Richard L.

2017-08-01

Coherent diffraction imaging (CDI) is a rapidly developing form of imaging that offers the potential of wavelength-limited resolution without image-forming lenses. In CDI, the intensity of the diffraction pattern is measured directly by the detector, and various iterative phase retrieval algorithms are used to "invert" the diffraction pattern and reconstruct a high-resolution image of the sample. However, there are certain requirements in CDI that must be met to reconstruct the object. Although most experiments are conducted in the "far-field"—or Fraunhofer—regime where the requirements are not as stringent, some experiments must be conducted in the "near field" where Fresnel diffraction must be considered. According to the derivation of Fresnel diffraction, successful reconstructions can only be obtained when the small-angle number, a derived quantity, is much less than one. We show, however, that it is not actually necessary to fulfill the small-angle condition. The Fresnel kernel well approximates the exact kernel in regions where the phase oscillates slowly, and in regions of fast oscillations, indicated by large A n , the error between kernels should be negligible due to stationary-phase arguments. We experimentally verify this conclusion with a helium neon laser setup and show that it should hold at x-ray wavelengths as well.

Performance improvements of binary diffractive structures via optimization of the photolithography and dry etch processes

NASA Astrophysics Data System (ADS)

Welch, Kevin; Leonard, Jerry; Jones, Richard D.

2010-08-01

Increasingly stringent requirements on the performance of diffractive optical elements (DOEs) used in wafer scanner illumination systems are driving continuous improvements in their associated manufacturing processes. Specifically, these processes are designed to improve the output pattern uniformity of off-axis illumination systems to minimize degradation in the ultimate imaging performance of a lithographic tool. In this paper, we discuss performance improvements in both photolithographic patterning and RIE etching of fused silica diffractive optical structures. In summary, optimized photolithographic processes were developed to increase critical dimension uniformity and featuresize linearity across the substrate. The photoresist film thickness was also optimized for integration with an improved etch process. This etch process was itself optimized for pattern transfer fidelity, sidewall profile (wall angle, trench bottom flatness), and across-wafer etch depth uniformity. Improvements observed with these processes on idealized test structures (for ease of analysis) led to their implementation in product flows, with comparable increases in performance and yield on customer designs.

In situ study of maize starch gelatinization under ultra-high hydrostatic pressure using X-ray diffraction.

PubMed

Yang, Zhi; Gu, Qinfen; Hemar, Yacine

2013-08-14

The gelatinization of waxy (very low amylose) and high-amylose maize starches by ultra-high hydrostatic pressure (up to 6 GPa) was investigated in situ using synchrotron X-ray powder diffraction on samples held in a diamond anvil cell (DAC). The starch pastes, made by mixing starch and water in a 1:1 ratio, were pressurized and measured at room temperature. X-ray diffraction pattern showed that at 2.7 GPa waxy starch, which displayed A-type XRD pattern at atmospheric pressure, exhibited a faint B-type-like pattern. The B-type crystalline structures of high-amylose starch were not affected even when 1.5 GPa pressure was applied. However, both waxy and high-amylose maize starches can be fully gelatinized at 5.9 GPa and 5.1 GPa, respectively. In the case of waxy maize starch, upon release of pressure (to atmospheric pressure) crystalline structure appeared as a result of amylopectin aggregation. Copyright © 2013 Elsevier Ltd. All rights reserved.

Coherent convergent-beam time-resolved X-ray diffraction

PubMed Central

Spence, John C. H.; Zatsepin, Nadia A.; Li, Chufeng

2014-01-01

The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic laser radiation of a free-electron X-ray laser is unsuitable. We discuss the possibility of obtaining single-shot, angle-integrated rocking curves from CCB patterns, and the dependence of the resulting patterns on the focused beam coordinate when the beam diameter is larger or smaller than a nanocrystal, or smaller than one unit cell. We show how structure factor phase information is provided at overlapping interfering orders and how a common phase origin between different shots may be obtained. Their use in refinement of the phase-sensitive intensity between overlapping orders is suggested. PMID:24914153

Apparatus and method for laser beam diagnosis

DOEpatents

Salmon, Jr., Joseph T.

1991-01-01

An apparatus and method is disclosed for accurate, real time monitoring of the wavefront curvature of a coherent laser beam. Knowing the curvature, it can be quickly determined whether the laser beam is collimated, or focusing (converging), or de-focusing (diverging). The apparatus includes a lateral interferometer for forming an interference pattern of the laser beam to be diagnosed. The interference pattern is imaged to a spatial light modulator (SLM), whose output is a coherent laser beam having an image of the interference pattern impressed on it. The SLM output is focused to obtain the far-field diffraction pattern. A video camera, such as CCD, monitors the far-field diffraction pattern, and provides an electrical output indicative of the shape of the far-field pattern. Specifically, the far-field pattern comprises a central lobe and side lobes, whose relative positions are indicative of the radius of curvature of the beam. The video camera's electrical output may be provided to a computer which analyzes the data to determine the wavefront curvature of the laser beam.

Apparatus and method for laser beam diagnosis

DOEpatents

Salmon, J.T. Jr.

1991-08-27

An apparatus and method are disclosed for accurate, real time monitoring of the wavefront curvature of a coherent laser beam. Knowing the curvature, it can be quickly determined whether the laser beam is collimated, or focusing (converging), or de-focusing (diverging). The apparatus includes a lateral interferometer for forming an interference pattern of the laser beam to be diagnosed. The interference pattern is imaged to a spatial light modulator (SLM), whose output is a coherent laser beam having an image of the interference pattern impressed on it. The SLM output is focused to obtain the far-field diffraction pattern. A video camera, such as CCD, monitors the far-field diffraction pattern, and provides an electrical output indicative of the shape of the far-field pattern. Specifically, the far-field pattern comprises a central lobe and side lobes, whose relative positions are indicative of the radius of curvature of the beam. The video camera's electrical output may be provided to a computer which analyzes the data to determine the wavefront curvature of the laser beam. 11 figures.

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

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

Balagurov, Anatoly M.; Bobrikov, Ivan A.; Bokuchava, Gizo D.

2015-11-15

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of themore » material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.« less

X-ray crystallography

NASA Technical Reports Server (NTRS)

2001-01-01

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

Determination of phase from the ridge of CWT using generalized Morse wavelet

NASA Astrophysics Data System (ADS)

Kocahan, Ozlem; Tiryaki, Erhan; Coskun, Emre; Ozder, Serhat

2018-03-01

The selection of wavelet is an important step in order to determine the phase from the fringe patterns. In the present work, a new wavelet for phase retrieval from the ridge of continuous wavelet transform (CWT) is presented. The phase distributions have been extracted from the optical fringe pattern by choosing the zero order generalized morse wavelet (GMW) as a mother wavelet. The aim of the study is to reveal the ways in which the two varying parameters of GMW affect the phase calculation. To show the validity of this method, an experimental study has been conducted by using the diffraction phase microscopy (DPM) setup; consequently, the profiles of red blood cells have been retrieved. The results for the CWT ridge technique with GMW have been compared with the results for the Morlet wavelet and the Paul wavelet; the results are almost identical for Paul and zero order GMW because of their degree of freedom. Also, for further discussion, the Fourier transform and the Stockwell transform have been applied comparatively. The outcome of the comparison reveals that GMWs are highly applicable to the research in various areas, predominantly biomedicine.

Kinetic precipitation of solution-phase polyoxomolybdate followed by transmission electron microscopy: a window to solution-phase nanostructure.

PubMed

Zhu, Yan; Cammers-Goodwin, Arthur; Zhao, Bin; Dozier, Alan; Dickey, Elizabeth C

2004-05-17

This study aimed to elucidate the structural nature of the polydisperse, nanoscopic components in the solution and the solid states of partially reduced polyoxomolybdate derived from the [Mo132] keplerate, [(Mo)Mo5]12-[Mo2 acetate]30. Designer tripodal hexamine-tris-crown ethers and nanoscopic molybdate coprecipitated from aqueous solution. These microcrystalline solids distributed particle radii between 2-30 nm as assayed by transmission electron microscopy (TEM). The solid materials and their particle size distributions were snap shots of the solution phase. The mother liquor of the preparation of the [Mo132] keplerate after three days revealed large species (r=20-30 nm) in the coprecipitate, whereas [Mo132] keplerate redissolved in water revealed small species (3-7 nm) in the coprecipitate. Nanoparticles of coprecipitate were more stable than solids derived solely from partially reduced molybdate. The TEM features of all material analyzed lacked facets on the nanometer length scale; however, the structures diffracted electrons and appeared to be defect-free as evidenced by Moiré patterns in the TEM images. Moiré patterns and size-invariant optical densities of the features in the micrographs suggested that the molybdate nanoparticles were vesicular.

Effect of bismuth doping on the structural and magnetic properties of zinc-ferrite nanoparticles prepared by a microwave combustion method

NASA Astrophysics Data System (ADS)

Shoushtari, Morteza Zargar; Emami, Akram; Ghahfarokhi, Seyed Ebrahim Mosavi

2016-12-01

In this study, we examine the bismuth doping effect on the structural, magnetic and microstructural properties of zinc-ferrite nanoparticles (ZnFe2-xBixO4 with x=0.0, 0.02, 0.04, 0.06, 0.1, 0.15) which have been prepared by a microwave combustion method. The structural, morphological and electromagnetic properties and also Curie temperature of the samples were examined by x-ray powder diffraction (XRD), field emission scanning electron microscope (FESEM), vibrating sample magnetometer (VSM), and LCR meter, respectively. In order to measure the energy band gap, the FTIR spectra of the samples were also considered. The XRD patterns of the samples revealed that all of them are ZnFe2O4 structure and no additional peak was observed in their patterns. This implied that the samples were single-phase up to bismuth solubility of 0.15 in Zinc-Ferrite. The results of XRD patterns also showed that the value lattice parameter increases with increasing the bismuth doping. The FESEM results revealed an ascending trend in the size of the nanoparticles. Also considering the VSM results characterized that an increasing the bismuth doping leads to lower the saturation magnetization. The Curie temperatures of the samples were reduced as a result of increasing the amount of bismuth.

Real-time x-ray diffraction measurements of shocked polycrystalline tin and aluminum.

PubMed

Morgan, Dane V; Macy, Don; Stevens, Gerald

2008-11-01

A new, fast, single-pulse x-ray diffraction (XRD) diagnostic for determining phase transitions in shocked polycrystalline materials has been developed. The diagnostic consists of a 37-stage Marx bank high-voltage pulse generator coupled to a needle-and-washer electron beam diode via coaxial cable, producing line and bremsstrahlung x-ray emission in a 35 ns pulse. The characteristic K(alpha) lines from the selected anodes of silver and molybdenum are used to produce the diffraction patterns, with thin foil filters employed to remove the characteristic K(beta) line emission. The x-ray beam passes through a pinhole collimator and is incident on the sample with an approximately 3 x 6 mm(2) spot and 1 degrees full width half maximum angular divergence in a Bragg-reflecting geometry. For the experiments described in this report, the angle between the incident beam and the sample surface was 8.5 degrees . A Debye-Scherrer diffraction image was produced on a phosphor located 76 mm from the polycrystalline sample surface. The phosphor image was coupled to a charge-coupled device camera through a coherent fiber-optic bundle. Dynamic single-pulse XRD experiments were conducted with thin foil samples of tin, shock loaded with a 1 mm vitreous carbon back window. Detasheet high explosive with a 2-mm-thick aluminum buffer was used to shock the sample. Analysis of the dynamic shock-loaded tin XRD images revealed a phase transformation of the tin beta phase into an amorphous or liquid state. Identical experiments with shock-loaded aluminum indicated compression of the face-centered-cubic aluminum lattice with no phase transformation.

Trapezoidal diffraction grating beam splitters in single crystal diamond

NASA Astrophysics Data System (ADS)

Kiss, Marcell; Graziosi, Teodoro; Quack, Niels

2018-02-01

Single Crystal Diamond has been recognized as a prime material for optical components in high power applications due to low absorption and high thermal conductivity. However, diamond microstructuring remains challenging. Here, we report on the fabrication and characterization of optical diffraction gratings exhibiting a symmetric trapezoidal profile etched into a single crystal diamond substrate. The optimized grating geometry diffracts the transmitted optical power into precisely defined proportions, performing as an effective beam splitter. We fabricate our gratings in commercially available single crystal CVD diamond plates (2.6mm x 2.6mm x 0.3mm). Using a sputter deposited hard mask and patterning by contact lithography, the diamond is etched in an inductively coupled oxygen plasma with zero platen power. The etch process effectively reveals the characteristic {111} diamond crystal planes, creating a precisely defined angled (54.7°) profile. SEM and AFM measurements of the fabricated gratings evidence the trapezoidal shape with a pitch of 3.82μm, depth of 170 nm and duty cycle of 35.5%. Optical characterization is performed in transmission using a 650nm laser source perpendicular to the sample. The recorded transmitted optical power as function of detector rotation angle shows a distribution of 21.1% in the 0th order and 23.6% in each +/-1st order (16.1% reflected, 16.6% in higher orders). To our knowledge, this is the first demonstration of diffraction gratings with trapezoidal profile in single crystal diamond. The fabrication process will enable beam splitter gratings of custom defined optical power distribution profiles, while antireflection coatings can increase the efficiency.

Influence of defect luminescence and structural modification on the electrical properties of Magnesium Doped Zinc Oxide Nanorods

NASA Astrophysics Data System (ADS)

Santoshkumar, B.; Biswas, Amrita; Kalyanaraman, S.; Thangavel, R.; Udayabhanu, G.; Annadurai, G.; Velumani, S.

2017-06-01

Magnesium doped zinc oxide nanorod arrays on zinc oxide seed layers were grown by hydrothermal method. X-ray diffraction (XRD) patterns revealed the growth orientation along the preferential (002) direction. The hexagonal morphology was revealed from the field emission scanning electron microscope (FESEM) images. The elemental composition of the samples was confirmed by energy dispersive x-ray analysis spectra (EDS) and mapping dots. Carrier concentration, resistivity and mobility of the samples were obtained by Hall measurements. I-V characteristic curve confirmed the increase in resistivity upon doping. Photoluminescence (PL) spectra exposed the characteristic of UV emission along with defect mediated visible emission in the samples. Electrochemical impedance spectroscopy and cyclic voltammetry were undertaken to study the charge transport property. Owing to the change in the structural parameters and defect concentration the electrical properties of the doped samples were altered.

Microwave-assisted synthesis and characterization of nickel ferrite nanoparticles

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

Carpenter, Gopal; Sen, Ravindra; Gupta, Nitish, E-mail: nitish.nidhi75@gmail.com

2015-08-28

Nickel ferrite nanoparticles (NiFe{sub 2}O{sub 4}) were successfully prepared by microwave-assisted combustion method (MWAC) using citric Electron acid as a chelating agent. NiFe{sub 2}O{sub 4} nanoparticles were characterized by X-ray diffraction (XRD) pattern, Scanning Microscopy (SEM), Fourier transform infrared (FTIR) and UV-Visible techniques. XRD analysis revealed that NiFe{sub 2}O{sub 4} nanoparticles have spinel cubic structure with the average crystalline size of 26.38 nm. SEM analysis revealed random and porous structural morphology of particles and FTIR showed absorption bands related to octahedral and tetrahedral sites, in the range 400–600cm{sup −1} which strongly favor the formation of NiFe{sub 2}O{sub 4} nanoparticles. The opticalmore » band gap is determined by UV Visible method and found to be 5.4 eV.« less

Synthesis of ZnO decorated graphene nanocomposite for enhanced photocatalytic properties

NASA Astrophysics Data System (ADS)

Gayathri, S.; Jayabal, P.; Kottaisamy, M.; Ramakrishnan, V.

2014-05-01

Zinc oxide/Graphene (GZ) composites with different concentrations of ZnO were successfully synthesized through simple chemical precipitation method. The X-ray diffraction pattern and the micro-Raman spectroscopic technique revealed the formation of GZ composite, and the energy dispersive X-ray spectrometry analysis showed the purity of the prepared samples. The ZnO nanoparticles decorated graphene sheets were clearly visible in the field emission scanning electron micrograph. Raman mapping was employed to analyze the homogeneity of the prepared samples. The diffuse-reflectance spectra clearly indicated that the formation of GZ composites promoted the absorption in the visible region also. The photocatalytic activity of ZnO and GZ composites was studied by the photodegradation of Methylene blue dye. The results revealed that the GZ composites exhibited a higher photocatalytic activity than pristine ZnO. Hence, we proposed a simple wet chemical method to synthesize GZ composite and its application on photocatalysis was demonstrated.

Hydrothermal growth of highly monodispersed TiO2 nanoparticles: Functional properties and dye-sensitized solar cell performance

NASA Astrophysics Data System (ADS)

Navaneethan, M.; Nithiananth, S.; Abinaya, R.; Harish, S.; Archana, J.; Sudha, L.; Ponnusamy, S.; Muthamizhchelvan, C.; Ikeda, H.; Hayakawa, Y.

2017-10-01

Monodispersed anatase TiO2 nanoparticles were synthesized by hydrothermal method using citric acid as a capping agent. The effect of citric acid and the growth time on the formation of TiO2, functional properties and dye-sensitized solar cell performances were investigated. X-ray diffraction pattern (XRD) and Raman spectroscopy results revealed that the TiO2 nanoparticles possess the anatase phase. Transmission electron microscopy (TEM) measurement revealed the formation of spherical nanoparticles with monodispersity in size and morphology. An average size of 14 nm was obtained for the growth period of 15 h. The maximum efficiency (η) of dye-sensitized solar cell was achieved for TiO2 nanoparticles grown for 15 h as 7.66% which was higher than that of commercial P25 TiO2 (5.23%) and uncapped nanoparticles (3.68%).

Properties of Nanocrystalline Cubic Silicon Carbide Thin Films Prepared by Hot-Wire Chemical Vapor Deposition Using SiH4/CH4/H2 at Various Substrate Temperatures

NASA Astrophysics Data System (ADS)

Tabata, Akimori; Komura, Yusuke; Hoshide, Yoshiki; Narita, Tomoki; Kondo, Akihiro

2008-01-01

Silicon carbide (SiC) thin films were prepared by hot-wire chemical vapor deposition from SiH4/CH4/H2 gases, and the influence of substrate temperature, Ts (104 < Ts < 434 °C), on the properties of the SiC thin films was investigated. X-ray diffraction patterns and Raman scattering spectra revealed that nanocrystalline cubic SiC (nc-3C-SiC) films grew at Ts above 187 °C, while completely amorphous films grew at Ts = 104 °C. Fourier transform infrared absorption spectra revealed that the crystallinity of the nc-3C-SiC was improved with increasing Ts up to 282 °C and remained almost unchanged with a further increase in Ts from 282 to 434 °C. The spin density was reduced monotonically with increasing Ts.

Third order nonlinear optical properties of Mn doped CeO2 nanostructures

NASA Astrophysics Data System (ADS)

Mani Rahulan, K.; Angeline Little Flower, N.; Annie Sujatha, R.; Mohana Priya, P.; Gopalakrishnan, C.

2018-05-01

Mn doped CeO2 nanoparticles with different ratios of Mn were synthesized by hydrothermal method and their structural properties were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Scanning electron microscopy (SEM). XRD patterns revealed that the peaks are highly crystalline structure with no segregation of Mn. The surface morphology from SEM reveals that particle size decreases with increase in Mn concentration. Nonlinear optical studies of the samples were measured by single-beam open aperture Z-scan technique using 5 ns laser pulses at 532 nm. The measured optical nonlinearity of all the samples exhibit typical third order nonlinear optical behavior including two-photon absorption (2 PA) and reverse saturable absorption (RSA). The experimental results show that the presence of RSA in these nanoparticles makes them a promising material for the fabrication of optical limiting devices. .

Relativistic electron diffraction at the UCLA Pegasus photoinjector laboratory.

PubMed

Musumeci, P; Moody, J T; Scoby, C M

2008-10-01

Electron diffraction holds the promise to yield real-time resolution of atomic motion in an easily accessible environment like a university laboratory at a fraction of the cost of fourth-generation X-ray sources. Currently the limit in time-resolution for conventional electron diffraction is set by how short an electron pulse can be made. A very promising solution to maintain the highest possible beam intensity without excessive pulse broadening from space charge effects is to increase the electron energy to the MeV level where relativistic effects significantly reduce the space charge forces. Rf photoinjectors can in principle deliver up to 10(7)-10(8) electrons packed in bunches of approximately 100-fs length, allowing an unprecedented time resolution and enabling the study of irreversible phenomena by single-shot diffraction patterns. The use of rf photoinjectors as sources for ultrafast electron diffraction has been recently at the center of various theoretical and experimental studies. The UCLA Pegasus laboratory, commissioned in early 2007 as an advanced photoinjector facility, is the only operating system in the country, which has recently demonstrated electron diffraction using a relativistic beam from an rf photoinjector. Due to the use of a state-of-the-art ultrashort photoinjector driver laser system, the beam has been measured to be sub-100-fs long, at least a factor of 5 better than what measured in previous relativistic electron diffraction setups. Moreover, diffraction patterns from various metal targets (titanium and aluminum) have been obtained using the Pegasus beam. One of the main laboratory goals in the near future is to fully develop the rf photoinjector-based ultrafast electron diffraction technique with particular attention to the optimization of the working point of the photoinjector in a low-charge ultrashort pulse regime, and to the development of suitable beam diagnostics.

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.

Optical Crystals

ERIC Educational Resources Information Center

Bergsten, Ronald

1974-01-01

Discusses the production and structure of a sequence of optical crystals which can serve as one-, two-, and three-dimensional diffraction plates to illustrate diffraction patterns by using light rather than x-rays or particles. Applications to qualitative presentations of Laue theory at the secondary and college levels are recommended. (CC)

Time-resolved measurements with streaked diffraction patterns from electrons generated in laser plasma wakefield

NASA Astrophysics Data System (ADS)

He, Zhaohan; Nees, John; Hou, Bixue; Krushelnick, Karl; Thomas, Alec; Beaurepaire, Benoît; Malka, Victor; Faure, Jérôme

2013-10-01

Femtosecond bunches of electrons with relativistic to ultra-relativistic energies can be robustly produced in laser plasma wakefield accelerators (LWFA). Scaling the electron energy down to sub-relativistic and MeV level using a millijoule laser system will make such electron source a promising candidate for ultrafast electron diffraction (UED) applications due to the intrinsic short bunch duration and perfect synchronization with the optical pump. Recent results of electron diffraction from a single crystal gold foil, using LWFA electrons driven by 8-mJ, 35-fs laser pulses at 500 Hz, will be presented. The accelerated electrons were collimated with a solenoid magnetic lens. By applying a small-angle tilt to the magnetic lens, the diffraction pattern can be streaked such that the temporal evolution is separated spatially on the detector screen after propagation. The observable time window and achievable temporal resolution are studied in pump-probe measurements of photo-induced heating on the gold foil.

Imaging single cells in a beam of live cyanobacteria with an X-ray laser.

PubMed

van der Schot, Gijs; Svenda, Martin; Maia, Filipe R N C; Hantke, Max; DePonte, Daniel P; Seibert, M Marvin; Aquila, Andrew; Schulz, Joachim; Kirian, Richard; Liang, Mengning; Stellato, Francesco; Iwan, Bianca; Andreasson, Jakob; Timneanu, Nicusor; Westphal, Daniel; Almeida, F Nunes; Odic, Dusko; Hasse, Dirk; Carlsson, Gunilla H; Larsson, Daniel S D; Barty, Anton; Martin, Andrew V; Schorb, Sebastian; Bostedt, Christoph; Bozek, John D; Rolles, Daniel; Rudenko, Artem; Epp, Sascha; Foucar, Lutz; Rudek, Benedikt; Hartmann, Robert; Kimmel, Nils; Holl, Peter; Englert, Lars; Duane Loh, Ne-Te; Chapman, Henry N; Andersson, Inger; Hajdu, Janos; Ekeberg, Tomas

2015-02-11

There exists a conspicuous gap of knowledge about the organization of life at mesoscopic levels. Ultra-fast coherent diffractive imaging with X-ray free-electron lasers can probe structures at the relevant length scales and may reach sub-nanometer resolution on micron-sized living cells. Here we show that we can introduce a beam of aerosolised cyanobacteria into the focus of the Linac Coherent Light Source and record diffraction patterns from individual living cells at very low noise levels and at high hit ratios. We obtain two-dimensional projection images directly from the diffraction patterns, and present the results as synthetic X-ray Nomarski images calculated from the complex-valued reconstructions. We further demonstrate that it is possible to record diffraction data to nanometer resolution on live cells with X-ray lasers. Extension to sub-nanometer resolution is within reach, although improvements in pulse parameters and X-ray area detectors will be necessary to unlock this potential.

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.

Effect of organic fuels on surface area and photocatalytic activity of scheelite CaWO4 nanoparticles

NASA Astrophysics Data System (ADS)

Manjunath, Kusuma; Gujjarahalli Thimmanna, Chandrappa

2018-03-01

Discrete nanoscale calcium tungstate (CaWO4) nanoparticles with exquisite photocatalytic activities were synthesized through ultra-rapid solution combustion route. Here, we aim to study the effect of different fuels on the synthesis of CaWO4 nanoparticles which lead to improve the characteristic properties and morphological evolution of the powders. From BET surface area measurement, it is observed that CaWO4 nanoparticles synthesized by using citric acid as fuel exhibits relatively large surface area (31.78 m2 g‑1) as compared to other fuels. The powder x-ray diffraction (PXRD) studies reveal that CaWO4 nanoparticles belong to scheelite type tetragonal system. The morphology of CaWO4 nanoparticles investigated using scanning electron microscopy (SEM) reveals that the powders are highly porous and agglomerated. Transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) images of the CaWO4 nanoparticles show that a well-dispersed nearly oval-shaped nanoparticles with variable dimensions and lattice spacing that depends on the type of fuels used in the synthesis. The selected area electron diffraction (SAED) patterns of CaWO4 nanoparticles exhibit several concentric rings with bright spots indicating the polycrystalline nature of the powders. Investigation on photocatalytic activity of CaWO4 nanoparticles synthesized using citric acid shows highest (∼93%) degradation of methylene blue (MB).

Direct observation of antisite defects in LiCoPO4 cathode materials by annular dark- and bright-field electron microscopy.

PubMed

Truong, Quang Duc; Devaraju, Murukanahally Kempaiah; Tomai, Takaaki; Honma, Itaru

2013-10-23

LiCoPO4 cathode materials have been synthesized by a sol-gel route. X-ray diffraction analysis confirmed that LiCoPO4 was well-crystallized in an orthorhombic structure in the Pmna space group. From the high-resolution transmission electron microscopy (HR-TEM) image, the lattice fringes of {001} and {100} are well-resolved. The HR-TEM image and selected area electron diffraction pattern reveal the highly crystalline nature of LiCoPO4 having an ordered olivine structure. The atom-by-atom structure of LiCoPO4 olivine has been observed, for the first time, using high-angle annular dark-field (HAADF) and annual bright-field scanning transmission electron microscopy. We observed the bright contrast in Li columns in the HAADF images and strong contrast in the ABF images, directly indicating the antisite exchange defects in which Co atoms partly occupy the Li sites. The LiCoPO4 cathode materials delivered an initial discharge capacity of 117 mAh/g at a C/10 rate with moderate cyclic performance. The discharge profile of LiCoPO4 shows a plateau at 4.75 V, revealing its importance as a potentially high-voltage cathode. The direct visualization of atom-by-atom structure in this work represents important information for the understanding of the structure of the active cathode materials for Li-ion batteries.

Structural characterization and evaluation of antioxidant, anticancer and hypoglycemic activity of radiation degraded oat (Avena sativa) β- glucan

NASA Astrophysics Data System (ADS)

Hussain, Peerzada R.; Rather, Sarver A.; Suradkar, Prashant P.

2018-03-01

Oat β-D-glucan after extraction was degraded at doses of 3, 6, 9, 12 and 15 kGy. The average molecular weight decreased to 45 kDa at dose of 15 kGy from an initial value of 200 kDa in native sample. XRD analysis revealed no significant change in diffraction pattern of irradiated samples when compared with control, except a decrease in intensity of x-ray diffraction. The results of the antioxidant activity revealed decrease in EC50 values and corresponding increase in antioxidant activity of radiation degraded oat β-D-glucan. Results of the anticancer studies indicated that cytotoxicity of gamma irradiated oat β-D-glucan in cancer cell lines was highest against colo-205 and MCF7 cancer cells compared to T47D cell and no cytotoxicity was observed in normal cell lines at all concentrations used. Evaluation of hypoglycemic activity showed highest inhibition in α-glucosidase activity compared to α-amylase activity due to gamma irradiation of oat β-D-glucan. Comparison of the EC50 values of known standards and gamma irradiated oat beta-glucan samples indicates that radiation treatment significantly modified the biological activity of the beta-glucan samples. Therefore, it is suggested that gamma irradiation can be used for producing low molecular weight oat β-D-glucan; which can help in modifying the biological activities.

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.

Diagnosis Applications of Non-Crystalline Diffraction of Collagen Fibres: Breast Cancer and Skin Diseases

NASA Astrophysics Data System (ADS)

Costa, M.; Benseny-Cases, N.; Cócera, M.; Teixeira, C. V.; Alsina, M.; Cladera, J.; López, O.; Fernández, M.; Sabés, M.

In previous chapters, the basis of SAXS for the study of biological systems like proteins in solution have been presented. The SAXS patterns of proteins in solution present, in general, broad dependences with the scattering vector, and the interpretation requires a huge component of modelling. In this chapter and in the following one, it is shown how SAXS technique can be used to study biological systems that are partially crystalline and with a large crystalline cells. This is done by analysing the diffraction obtained from these systems at small angles. In this chapter, a new approach to the application of small-angle X-ray scattering (SAXS) for diagnosis using the diffraction pattern of collagen is presented. This chapter shows the development of a new strategy in the preventive diagnosis of breast cancer following changes on collagen from breast connective tissue. SAXS profiles are related to different features in cutaneous preparations and to the supra-molecular arrangement of skin layers (stratum corneum, epidermis and dermis), in order to introduce objective values on the diagnosis of different skin pathologies. Working parameters (size, thickness) and methods (freezing, paraffin embedment) have been established. The results suggest that collagen diffraction patterns could be used as diagnostic indicators; especially for breast cancer and preliminary results obtained with skin collagen are promising too.

A structural investigation into the compaction behavior of pharmaceutical composites using powder X-ray diffraction and total scattering analysis.

PubMed

Moore, Michael D; Steinbach, Alison M; Buckner, Ira S; Wildfong, Peter L D

2009-11-01

To use advanced powder X-ray diffraction (PXRD) to characterize the structure of anhydrous theophylline following compaction, alone, and as part of a binary mixture with either alpha-lactose monohydrate or microcrystalline cellulose. Compacts formed from (1) pure theophylline and (2) each type of binary mixture were analyzed intact using PXRD. A novel mathematical technique was used to accurately separate multi-component diffraction patterns. The pair distribution function (PDF) of isolated theophylline diffraction data was employed to assess structural differences induced by consolidation and evaluated by principal components analysis (PCA). Changes induced in PXRD patterns by increasing compaction pressure were amplified by the PDF. Simulated data suggest PDF dampening is attributable to molecular deviations from average crystalline position. Samples compacted at different pressures were identified and differentiated using PCA. Samples compacted at common pressures exhibited similar inter-atomic correlations, where excipient concentration factored in the analyses involving lactose. Practical real-space structural analysis of PXRD data by PDF was accomplished for intact, compacted crystalline drug with and without excipient. PCA was used to compare multiple PDFs and successfully differentiated pattern changes consistent with compaction-induced disordering of theophylline as a single component and in the presence of another material.

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.

Domain alignment within ferroelectric/dielectric PbTiO 3 /SrTiO 3 superlattice nanostructures

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

Park, Joonkyu; Mangeri, John; Zhang, Qingteng

The ferroelectric domain pattern within lithographically defined PbTiO 3/SrTiO 3 ferroelectric/dielectric heteroepitaxial superlattice nanostructures is strongly influenced by the edges of the structures. Synchrotron X-ray nanobeam diffraction reveals that the spontaneously formed 180° ferroelectric stripe domains exhibited by such superlattices adopt a configuration in rectangular nanostructures in which domain walls are aligned with long patterned edges. The angular distribution of X-ray diffuse scattering intensity from nanodomains indicates that domains are aligned within an angular range of approximately 20° with respect to the edges. Computational studies based on a time-dependent Landau–Ginzburg–Devonshire model show that the preferred direction of the alignment resultsmore » from lowering of the bulk and electrostrictive contributions to the free energy of the system due to the release of the lateral mechanical constraint. This unexpected alignment appears to be intrinsic and not a result of distortions or defects caused by the patterning process. Thus, our work demonstrates how nanostructuring and patterning of heteroepitaxial superlattices allow for pathways to create and control ferroelectric structures that may appear counterintuitive.« less

Domain alignment within ferroelectric/dielectric PbTiO 3 /SrTiO 3 superlattice nanostructures

DOE PAGES

Park, Joonkyu; Mangeri, John; Zhang, Qingteng; ...

2018-01-22

The ferroelectric domain pattern within lithographically defined PbTiO 3/SrTiO 3 ferroelectric/dielectric heteroepitaxial superlattice nanostructures is strongly influenced by the edges of the structures. Synchrotron X-ray nanobeam diffraction reveals that the spontaneously formed 180° ferroelectric stripe domains exhibited by such superlattices adopt a configuration in rectangular nanostructures in which domain walls are aligned with long patterned edges. The angular distribution of X-ray diffuse scattering intensity from nanodomains indicates that domains are aligned within an angular range of approximately 20° with respect to the edges. Computational studies based on a time-dependent Landau–Ginzburg–Devonshire model show that the preferred direction of the alignment resultsmore » from lowering of the bulk and electrostrictive contributions to the free energy of the system due to the release of the lateral mechanical constraint. This unexpected alignment appears to be intrinsic and not a result of distortions or defects caused by the patterning process. Thus, our work demonstrates how nanostructuring and patterning of heteroepitaxial superlattices allow for pathways to create and control ferroelectric structures that may appear counterintuitive.« less

Image-based spectroscopy for environmental monitoring

NASA Astrophysics Data System (ADS)

Bachmakov, Eduard; Molina, Carolyn; Wynne, Rosalind

2014-03-01

An image-processing algorithm for use with a nano-featured spectrometer chemical agent detection configuration is presented. The spectrometer chip acquired from Nano-Optic DevicesTM can reduce the size of the spectrometer down to a coin. The nanospectrometer chip was aligned with a 635nm laser source, objective lenses, and a CCD camera. The images from a nanospectrometer chip were collected and compared to reference spectra. Random background noise contributions were isolated and removed from the diffraction pattern image analysis via a threshold filter. Results are provided for the image-based detection of the diffraction pattern produced by the nanospectrometer. The featured PCF spectrometer has the potential to measure optical absorption spectra in order to detect trace amounts of contaminants. MATLAB tools allow for implementation of intelligent, automatic detection of the relevant sub-patterns in the diffraction patterns and subsequent extraction of the parameters using region-detection algorithms such as the generalized Hough transform, which detects specific shapes within the image. This transform is a method for detecting curves by exploiting the duality between points on a curve and parameters of that curve. By employing this imageprocessing technique, future sensor systems will benefit from new applications such as unsupervised environmental monitoring of air or water quality.

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

Meng, Yifei; Zuo, Jian -Min

A diffraction-based technique is developed for the determination of three-dimensional nanostructures. The technique employs high-resolution and low-dose scanning electron nanodiffraction (SEND) to acquire three-dimensional diffraction patterns, with the help of a special sample holder for large-angle rotation. Grains are identified in three-dimensional space based on crystal orientation and on reconstructed dark-field images from the recorded diffraction patterns. Application to a nanocrystalline TiN thin film shows that the three-dimensional morphology of columnar TiN grains of tens of nanometres in diameter can be reconstructed using an algebraic iterative algorithm under specified prior conditions, together with their crystallographic orientations. The principles can bemore » extended to multiphase nanocrystalline materials as well. Furthermore, the tomographic SEND technique provides an effective and adaptive way of determining three-dimensional nanostructures.« less

A versatile diffractive maskless lithography for single-shot and serial microfabrication.

PubMed

Jenness, Nathan J; Hill, Ryan T; Hucknall, Angus; Chilkoti, Ashutosh; Clark, Robert L

2010-05-24

We demonstrate a diffractive maskless lithographic system that is capable of rapidly performing both serial and single-shot micropatterning. Utilizing the diffractive properties of phase holograms displayed on a spatial light modulator, arbitrary intensity distributions were produced to form two and three dimensional micropatterns/structures in a variety of substrates. A straightforward graphical user interface was implemented to allow users to load templates and change patterning modes within the span of a few minutes. A minimum resolution of approximately 700 nm is demonstrated for both patterning modes, which compares favorably to the 232 nm resolution limit predicted by the Rayleigh criterion. The presented method is rapid and adaptable, allowing for the parallel fabrication of microstructures in photoresist as well as the fabrication of protein microstructures that retain functional activity.

The Powder Diffraction File: Past, Present, and Future

PubMed Central

Smith, Deane K.; Jenkins, Ron

1996-01-01

The Powder Diffraction file has been the primary reference for Powder Diffraction Data for more than half a century. The file is a collection of about 65 000 reduced powder patterns stored as sets of d/I data along with the appropriate crystallographic, physical and experimental information. This paper reviews the development and growth of the PDF and discusses the role of the ICDD in the maintenance and dissemination of the file. PMID:27805163

Diffracted wavefield by an arbitrary aperture from Maggi-Rubinowicz transformation

NASA Astrophysics Data System (ADS)

Ganci, S.

2008-01-01

Fraunhofer diffraction patterns through apertures in opaque screens are the cases of most interest in optics. The major purpose of this paper is to establish a general and explicit formula for calculating diffracted wavefield from Maggi-Rubinowicz transformation. The 2-D integration (Rayleigh-Sommerfeld or Helmholtz-Kirchhoff integral formulas) is reduced to a 1-D integration over the rim of the aperture. Some examples for elliptical and polygonal apertures are given.

X-ray diffraction from nonuniformly stretched helical molecules

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

Prodanovic, Momcilo; Irving, Thomas C.; Mijailovich, Srboljub M.

2016-04-18

The fibrous proteins in living cells are exposed to mechanical forces interacting with other subcellular structures. X-ray fiber diffraction is often used to assess deformation and movement of these proteins, but the analysis has been limited to the theory for fibrous molecular systems that exhibit helical symmetry. However, this approach cannot adequately interpret X-ray data from fibrous protein assemblies where the local strain varies along the fiber length owing to interactions of its molecular constituents with their binding partners. To resolve this problem a theoretical formulism has been developed for predicting the diffraction from individual helical molecular structures nonuniformly strainedmore » along their lengths. This represents a critical first step towards modeling complex dynamical systems consisting of multiple helical structures using spatially explicit, multi-scale Monte Carlo simulations where predictions are compared with experimental data in a `forward' process to iteratively generate ever more realistic models. Here the effects of nonuniform strains and the helix length on the resulting magnitude and phase of diffraction patterns are quantitatively assessed. Examples of the predicted diffraction patterns of nonuniformly deformed double-stranded DNA and actin filaments in contracting muscle are presented to demonstrate the feasibly of this theoretical approach.« less

A Novel In-situ Electrochemical Cell for Neutron Diffraction Studies of Phase Transitions in Small Volume Electrodes of Li-ion Batteries

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

Vadlamani, Bhaskar S; An, Ke; Jagannathan, M.

2014-01-01

The design and performance of a novel in-situ electrochemical cell that greatly facilitates the neutron diffraction study of complex phase transitions in small volume electrodes of Li-ion cells, is presented in this work. Diffraction patterns that are Rietveld-refinable could be obtained simultaneously for all the electrodes, which demonstrates that the cell is best suited to explore electrode phase transitions driven by the lithiation and delithiation processes. This has been facilitated by the use of single crystal (100) Si sheets as casing material and the planar cell configuration, giving improved signal-to-noise ratio relative to other casing materials. The in-situ cell hasmore » also been designed for easy assembly and to facilitate rapid experiments. The effectiveness of cell is demonstrated by tracking the neutron diffraction patterns during the charging of graphite/LiCoO2 and graphite/LiMn2O4 cells. It is shown that good quality neutron diffraction data can be obtained and that most of the finer details of the phase transitions, and the associated changes in crystallographic parameters in these electrodes, can be captured.« less

Improved crystal orientation and physical properties from single-shot XFEL stills

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

Sauter, Nicholas K., E-mail: nksauter@lbl.gov; Hattne, Johan; Brewster, Aaron S.

X-ray free-electron laser crystallography relies on the collection of still-shot diffraction patterns. New methods are developed for optimal modeling of the crystals’ orientations and mosaic block properties. X-ray diffraction patterns from still crystals are inherently difficult to process because the crystal orientation is not uniquely determined by measuring the Bragg spot positions. Only one of the three rotational degrees of freedom is directly coupled to spot positions; the other two rotations move Bragg spots in and out of the reflecting condition but do not change the direction of the diffracted rays. This hinders the ability to recover accurate structure factorsmore » from experiments that are dependent on single-shot exposures, such as femtosecond diffract-and-destroy protocols at X-ray free-electron lasers (XFELs). Here, additional methods are introduced to optimally model the diffraction. The best orientation is obtained by requiring, for the brightest observed spots, that each reciprocal-lattice point be placed into the exact reflecting condition implied by Bragg’s law with a minimal rotation. This approach reduces the experimental uncertainties in noisy XFEL data, improving the crystallographic R factors and sharpening anomalous differences that are near the level of the noise.« less

Light Diffraction by Large Amplitude Ultrasonic Waves in Liquids

NASA Technical Reports Server (NTRS)

Adler, Laszlo; Cantrell, John H.; Yost, William T.

2016-01-01

Light diffraction from ultrasound, which can be used to investigate nonlinear acoustic phenomena in liquids, is reported for wave amplitudes larger than that typically reported in the literature. Large amplitude waves result in waveform distortion due to the nonlinearity of the medium that generates harmonics and produces asymmetries in the light diffraction pattern. For standing waves with amplitudes above a threshold value, subharmonics are generated in addition to the harmonics and produce additional diffraction orders of the incident light. With increasing drive amplitude above the threshold a cascade of period-doubling subharmonics are generated, terminating in a region characterized by a random, incoherent (chaotic) diffraction pattern. To explain the experimental results a toy model is introduced, which is derived from traveling wave solutions of the nonlinear wave equation corresponding to the fundamental and second harmonic standing waves. The toy model reduces the nonlinear partial differential equation to a mathematically more tractable nonlinear ordinary differential equation. The model predicts the experimentally observed cascade of period-doubling subharmonics terminating in chaos that occurs with increasing drive amplitudes above the threshold value. The calculated threshold amplitude is consistent with the value estimated from the experimental data.

Synthesis, Characterization, and Antibacterial Activity of Cross-Linked Chitosan-Glutaraldehyde

PubMed Central

Li, Bin; Shan, Chang-Lin; Zhou, Qing; Fang, Yuan; Wang, Yang-Li; Xu, Fei; Han, Li-Rong; Ibrahim, Muhammad; Guo, Long-Biao; Xie, Guan-Lin; Sun, Guo-Chang

2013-01-01

This present study deals with synthesis, characterization and antibacterial activity of cross-linked chitosan-glutaraldehyde. Results from this study indicated that cross-linked chitosan-glutaraldehyde markedly inhibited the growth of antibiotic-resistant Burkholderia cepacia complex regardless of bacterial species and incubation time while bacterial growth was unaffected by solid chitosan. Furthermore, high temperature treated cross-linked chitosan-glutaraldehyde showed strong antibacterial activity against the selected strain 0901 although the inhibitory effects varied with different temperatures. In addition, physical-chemical and structural characterization revealed that the cross-linking of chitosan with glutaraldehyde resulted in a rougher surface morphology, a characteristic Fourier transform infrared (FTIR) band at 1559 cm−1, a specific X-ray diffraction peak centered at 2θ = 15°, a lower contents of carbon, hydrogen and nitrogen, and a higher stability of glucose units compared to chitosan based on scanning electron microscopic observation, FTIR spectra, X-ray diffraction pattern, as well as elemental and thermo gravimetric analysis. Overall, this study indicated that cross-linked chitosan-glutaraldehyde is promising to be developed as a new antibacterial drug. PMID:23670533

Synthesis of TiO2 Nanoparticle and its phase Transition

NASA Astrophysics Data System (ADS)

Mangrola, M. H.; Joshi, V. G.; Parmar, B. H.

2011-12-01

Here we report the synthesis of titanium dioxide (TiO2) nanoparticles and study of its phase transition from anataze to rutile. Titanium dioxide (TiO2) nanoparticles have been prepared by hydrolysis of Titanium isopropoxide an aqueous solution with constant value of pH 2 and peptizing the resultant suspension gel(white-Blue) and calcinate gel at different temperature. Structures of synthetic samples of TiO2 have been examined by X-ray diffraction (XRD) and scanning electron microscope (SEM). The anatase-rutile transition has been a popular topic due to its interest to scientific and engineering fields. . Here we have seen that the 100 °C calcinate powder consist of anatase fine crystalline phase with a particle size 14 to 15 nm. The prepared TiO2 nanoparticles have uniform size and morphology, and the phase transformation kinetics of obtained material was studied by interpretation of the X-ray diffraction patterns peaks. The phase transform occurred from anatase to rutile at calcinate temperature up to 600 °C. A very fine network texture made from uniform nanoparticles was revealed by scanning electron microscopy (SEM) analyses.

Dislocation structure in textured zirconium tensile-deformed along rolling and transverse directions determined by X-ray diffraction line profile analysis

NASA Astrophysics Data System (ADS)

Fan, Zhijian; Jóni, Bertalan; Xie, Lei; Ribárik, Gábor; Ungár, Tamás

2018-04-01

Specimens of cold-rolled zirconium were tensile-deformed along the rolling (RD) and the transverse (TD) directions. The stress-strain curves revealed a strong texture dependence. High resolution X-ray line profile analysis was used to determine the prevailing active slip-systems in the specimens with different textures. The reflections in the X-ray diffraction patterns were separated into two groups. One group corresponds to the major and the other group to the random texture component, respectively. The dislocation densities, the subgrain size and the prevailing active slip-systems were evaluated by using the convolutional multiple whole profile (CMWP) procedure. These microstructure parameters were evaluated separately in the two groups of reflections corresponding to the two different texture components. Significant differences were found in both, the evolution of dislocation densities and the development of the fractions of and type slip systems in the RD and TD specimens during tensile deformation. The differences between the RD and TD stress-strain curves are discussed in terms of the differences of the microstructure evolution.

Resonant x-ray diffraction revealing chemical disorder in sputtered L10 FeNi on Si(0 0 1)

NASA Astrophysics Data System (ADS)

Frisk, Andreas; Lindgren, Bengt; Pappas, Spiridon D.; Johansson, Erik; Andersson, Gabriella

2016-10-01

In the search for new rare earth free permanent magnetic materials, FeNi with a L10 structure is a possible candidate. We have synthesized the phase in the thin film form by sputtering onto HF-etched Si(0 0 1) substrates. Monatomic layers of Fe and Ni were alternately deposited on a Cu buffer layer, all of which grew epitaxially on the Si substrates. A good crystal structure and epitaxial relationship was confirmed by in-house x-ray diffraction (XRD). The chemical order, which to some part is the origin of an uniaxial magnetic anisotropy, was measured by resonant XRD. The 0 0 1 superlattice reflection was split in two symmetrically spaced peaks due to a composition modulation of the Fe and Ni layers. Furthermore the influence of roughness induced chemical anti-phase domains on the RXRD pattern is exemplified. A smaller than expected magnetic uniaxial anisotropy energy was obtained, which is partly due to the composition modulations, but the major reason is concluded to be the Cu buffer surface roughness.

Resonant x-ray diffraction revealing chemical disorder in sputtered L10 FeNi on Si(0 0 1).

PubMed

Frisk, Andreas; Lindgren, Bengt; Pappas, Spiridon D; Johansson, Erik; Andersson, Gabriella

2016-10-12

In the search for new rare earth free permanent magnetic materials, FeNi with a L10 structure is a possible candidate. We have synthesized the phase in the thin film form by sputtering onto HF-etched Si(0 0 1) substrates. Monatomic layers of Fe and Ni were alternately deposited on a Cu buffer layer, all of which grew epitaxially on the Si substrates. A good crystal structure and epitaxial relationship was confirmed by in-house x-ray diffraction (XRD). The chemical order, which to some part is the origin of an uniaxial magnetic anisotropy, was measured by resonant XRD. The 0 0 1 superlattice reflection was split in two symmetrically spaced peaks due to a composition modulation of the Fe and Ni layers. Furthermore the influence of roughness induced chemical anti-phase domains on the RXRD pattern is exemplified. A smaller than expected magnetic uniaxial anisotropy energy was obtained, which is partly due to the composition modulations, but the major reason is concluded to be the Cu buffer surface roughness.

Hydrothermal synthesis and characterization of hydroxyapatite and fluorhydroxyapatite nano-size powders.

PubMed

Montazeri, Leila; Javadpour, Jafar; Shokrgozar, Mohammad Ali; Bonakdar, Shahin; Javadian, Sayfoddin

2010-08-01

Pure hydroxyapatite (HAp) and fluoride-containing apatite powders (FHAp) were synthesized using a hydrothermal method. The powders were assessed by x-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscope (SEM) and F-selective electrode. X-ray diffraction results revealed the formation of single phase apatite structure for all the compositions synthesized in this work. However, the addition of a fluoride ion led to a systematic shift in the (3 0 0) peak of the XRD pattern as well as modifications in the FTIR spectra. It was found that the efficiency of fluoride ion incorporation decreased with the increase in the fluoride ion content. Fluorine incorporation efficiency was around 60% for most of the FHAp samples prepared in the current study. Smaller and less agglomerated particles were obtained by fluorine substitution. The bioactivity of the powder samples with different fluoride contents was compared by performing cell proliferation, alkaline phosphatase (ALP) and Alizarin red staining assays. Human osteoblast cells were used to assess the cellular responses to the powder samples in this study. Results demonstrated a strong dependence of different cell activities on the level of fluoridation.

Periodic Grating-like Patterns Induced by Self-Assembly of Gelator Fibres in Nematic Gels.

PubMed

Topnani, Neha B; Prutha, N; Pratibha, R

2018-03-15

Periodic orientation patterns occurring in nematic gels, revealed by optical and scanning electron microscopy, are found to be formed by spontaneous self-assembly of fibrous aggregates of a low-molecular-weight organogelator in an aligned thermotropic liquid crystal (LC). Self-organization into periodic structures is also reflected in a calorimetric study, which shows the occurrence of three thermoreversible states, namely, isotropic liquid, nematic and nematic gel. The segregation and self-assembly of the fibrous aggregates leading to pattern formation are attributed to the highly polar LC and to hydrogen bonding between gelator molecules, as shown by X-ray diffraction and vibrational spectroscopy. This study aims to investigate in detail the effect of the chemical nature and alignment of an anisotropic solvent on the morphology of the gelator fibres and the resulting gelation process. The periodic organization of LC-rich and fibre-rich regions can also provide a way to obtain templates for positioning nanoparticle arrays in an LC matrix, which can lead to novel devices. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effects of annealing on arrays of Ge nanocolumns formed by glancing angle deposition

NASA Astrophysics Data System (ADS)

Khare, C.; Gerlach, J. W.; Höche, T.; Fuhrmann, B.; Leipner, H. S.; Rauschenbach, B.

2012-10-01

Post-deposition thermal annealing of glancing angle deposited Ge nanocolumn arrays was carried out in a continuous Ar-flow at temperatures ranging from TA = 300 to 800 °C for different annealing durations. Morphological alterations and the recrystallization process induced by the thermal annealing treatment were investigated for the Ge nanocolumns deposited on planar and pre-patterned Si substrates. From X-ray diffraction (XRD) measurements, the films annealed at TA ≥ 500 °C were found to be polycrystalline. On planar Si substrates, at TA = 600 °C nanocolumns exhibited strong coarsening and merging, while a complete disintegration of the nanocolumns was detected at TA = 700 °C. The morphology of nanostructures deposited on pre-patterned substrates differs substantially, where the merging or column-disintegration effect was absent at elevated annealing temperatures. The two-arm-chevron nanostructures grown on pre-patterned substrates retained their complex shape and morphology, after extended annealing intervals. Investigations by transmission electron microscopy revealed nanocrystalline domains of the order of 5-30 nm (in diameter) present within the chevron structures after the annealing treatment.

Achromatic shearing phase sensor for generating images indicative of measure(s) of alignment between segments of a segmented telescope's mirrors

NASA Technical Reports Server (NTRS)

Stahl, H. Philip (Inventor); Walker, Chanda Bartlett (Inventor)

2006-01-01

An achromatic shearing phase sensor generates an image indicative of at least one measure of alignment between two segments of a segmented telescope's mirrors. An optical grating receives at least a portion of irradiance originating at the segmented telescope in the form of a collimated beam and the collimated beam into a plurality of diffraction orders. Focusing optics separate and focus the diffraction orders. Filtering optics then filter the diffraction orders to generate a resultant set of diffraction orders that are modified. Imaging optics combine portions of the resultant set of diffraction orders to generate an interference pattern that is ultimately imaged by an imager.

Microscale optical cryptography using a subdiffraction-limit optical key

NASA Astrophysics Data System (ADS)

Ogura, Yusuke; Aino, Masahiko; Tanida, Jun

2018-04-01

We present microscale optical cryptography using a subdiffraction-limit optical pattern, which is finer than the diffraction-limit size of the decrypting optical system, as a key and a substrate with a reflectance distribution as an encrypted image. Because of the subdiffraction-limit spatial coding, this method enables us to construct a secret image with the diffraction-limit resolution. Simulation and experimental results demonstrate, both qualitatively and quantitatively, that the secret image becomes recognizable when and only when the substrate is illuminated with the designed key pattern.

Three-dimensional reconstruction of the giant mimivirus particle with an x-ray free-electron laser.

PubMed

Ekeberg, Tomas; Svenda, Martin; Abergel, Chantal; Maia, Filipe R N C; Seltzer, Virginie; Claverie, Jean-Michel; Hantke, Max; Jönsson, Olof; Nettelblad, Carl; van der Schot, Gijs; Liang, Mengning; DePonte, Daniel P; Barty, Anton; Seibert, M Marvin; Iwan, Bianca; Andersson, Inger; Loh, N Duane; Martin, Andrew V; Chapman, Henry; Bostedt, Christoph; Bozek, John D; Ferguson, Ken R; Krzywinski, Jacek; Epp, Sascha W; Rolles, Daniel; Rudenko, Artem; Hartmann, Robert; Kimmel, Nils; Hajdu, Janos

2015-03-06

We present a proof-of-concept three-dimensional reconstruction of the giant mimivirus particle from experimentally measured diffraction patterns from an x-ray free-electron laser. Three-dimensional imaging requires the assembly of many two-dimensional patterns into an internally consistent Fourier volume. Since each particle is randomly oriented when exposed to the x-ray pulse, relative orientations have to be retrieved from the diffraction data alone. We achieve this with a modified version of the expand, maximize and compress algorithm and validate our result using new methods.

Retrieval of the atomic displacements in the crystal from the coherent X-ray diffraction pattern.

PubMed

Minkevich, A A; Köhl, M; Escoubas, S; Thomas, O; Baumbach, T

2014-07-01

The retrieval of spatially resolved atomic displacements is investigated via the phases of the direct(real)-space image reconstructed from the strained crystal's coherent X-ray diffraction pattern. It is demonstrated that limiting the spatial variation of the first- and second-order spatial displacement derivatives improves convergence of the iterative phase-retrieval algorithm for displacements reconstructions to the true solution. This approach is exploited to retrieve the displacement in a periodic array of silicon lines isolated by silicon dioxide filled trenches.

Serial number coding and decoding by laser interference direct patterning on the original product surface for anti-counterfeiting.

PubMed

Park, In-Yong; Ahn, Sanghoon; Kim, Youngduk; Bae, Han-Sung; Kang, Hee-Shin; Yoo, Jason; Noh, Jiwhan

2017-06-26

Here, we investigate a method to distinguish the counterfeits by patterning multiple reflective type grating directly on the surface of the original product and analyze the serial number from its rotation angles of diffracted fringes. The micro-sized gratings were fabricated on the surface of the material at high speeds by illuminating the interference fringe generated by passing a high-energy pulse laser through the Fresnel biprism. In addition, analysis of the grating's diffraction fringes was performed using a continuous wave laser.

Structured illumination to spatially map chromatin motions.

PubMed

Bonin, Keith; Smelser, Amanda; Moreno, Naike Salvador; Holzwarth, George; Wang, Kevin; Levy, Preston; Vidi, Pierre-Alexandre

2018-05-01

We describe a simple optical method that creates structured illumination of a photoactivatable probe and apply this method to characterize chromatin motions in nuclei of live cells. A laser beam coupled to a diffractive optical element at the back focal plane of an excitation objective generates an array of near diffraction-limited beamlets with FWHM of 340  ±  30  nm, which simultaneously photoactivate a 7  ×  7 matrix pattern of GFP-labeled histones, with spots 1.70  μm apart. From the movements of the photoactivated spots, we map chromatin diffusion coefficients at multiple microdomains of the cell nucleus. The results show correlated motions of nearest chromatin microdomain neighbors, whereas chromatin movements are uncorrelated at the global scale of the nucleus. The method also reveals a DNA damage-dependent decrease in chromatin diffusion. The diffractive optical element instrumentation can be easily and cheaply implemented on commercial inverted fluorescence microscopes to analyze adherent cell culture models. A protocol to measure chromatin motions in nonadherent human hematopoietic stem and progenitor cells is also described. We anticipate that the method will contribute to the identification of the mechanisms regulating chromatin mobility, which influences most genomic processes and may underlie the biogenesis of genomic translocations associated with hematologic malignancies. (2018) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE).

A large format in operando wound cell for analysing the structural dynamics of lithium insertion materials

NASA Astrophysics Data System (ADS)

Brant, William R.; Roberts, Matthew; Gustafsson, Torbjörn; Biendicho, Jordi Jacas; Hull, Stephen; Ehrenberg, Helmut; Edström, Kristina; Schmid, Siegbert

2016-12-01

This paper presents a large wound cell for in operando neutron diffraction (ND) from which high quality diffraction patterns are collected every 15 min while maintaining conventional electrochemical performance. Under in operando data collection conditions the oxygen atomic displacement parameters (ADPs) and cell parameters were extracted for Li0.18Sr0.66Ti0.5Nb0.5O3. Analysis of diffraction data collected under in situ conditions revealed that the lithium is located on the (0.5 0.5 0) site, corresponding to the 3c Wyckoff position in the cubic perovskite unit cell, after the cell is discharged to 1 V. When the cell is discharged under potentiostatic conditions the quantity of lithium on this site increases, indicating a potential position where lithium becomes pinned in the thermodynamically stable phase. During this potentiostatic step the oxygen ADPs reduce significantly. On discharge, however, the oxygen ADPs were observed to increase gradually as more lithium is inserted into the structure. Finally, the rate of unit cell expansion changed by ∼44% once the lithium content approached ∼0.17 Li per formula unit. A link between lithium content and degree of mobility, disorder of the oxygen positions and changing rate of unit cell expansion at various stages during lithium insertion and extraction is thus presented.

Optical and Luminescence Properties of β-NaFeO2 Nanoparticles

NASA Astrophysics Data System (ADS)

Singh, Sarbjit; Tangra, Ankush Kumar; Lotey, Gurmeet Singh

2018-05-01

β-NaFeO2 nanoparticles have been synthesized by sol-gel method and their morphological, structural and optical properties investigated. Transmission electron microscope study reveals that the size of the synthesis nanoparticles is 37 nm and they are possessing spherical symmetry. X-ray diffraction pattern shows the orthorhombic crystal structure of nanoparticles with space group Pn21 a. UV-visible spectra of β-NaFeO2 divulges that these nanoparticles have direct band gap 2.35 eV. The observed Fourier transform infrared spectroscopy spectra confirms the presence of Fe-Na bonding at 1074 cm-1. The photoluminescence study of these nanoparticles shows that these nanoparticles possesses various transition in the visible spectrum.