Crystallites

Distribution by Scientific Domains
Distribution within Polymers and Materials Science

Terms modified by Crystallites

  • crystallite orientation
  • crystallite size
  • crystallite size distribution

  • Selected Abstracts


    Crystallite and Grain-Size-Dependent Phase Transformations in Yttria-Doped Zirconia

    JOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 2 2003
    Arun Suresh
    In pure zirconia, ultrafine powders are often observed to take on the high-temperature tetragonal phase instead of the "equilibrium" monoclinic phase. The present experiments and analysis show that this observation is one manifestation of a much more general phenomenon in which phase transformation temperatures shift with crystallite/grain size. In the present study, the effect of crystallite (for powders) and grain (for solids) size on the tetragonal , monoclinic phase transformation is examined more broadly across the yttria,zirconia system. Using dilatometry and high-temperature differential scanning calorimetry on zirconia samples with varying crystallite/grain sizes and yttria content, we are able to show that the tetragonal , monoclinic phase transformation temperature varies linearly with inverse crystallite/grain size. This experimental behavior is consistent with thermodynamic predictions that incorporate a surface energy difference term in the calculation of free-energy equilibrium between two phases. [source]


    Catalytic Reactions on Crystallites

    IMAGING & MICROSCOPY (ELECTRONIC), Issue 1 2006
    Imaging, In-situ Chemical Probing at the Nanometer Scale
    FIM and PFDMS are used for studying particles that mimic catalytic grains. Exposing tips to reactive gas mixtures allows following in-situ catalytic reactions on the nanometer scale. These techniques appear as unique tools to approach simultaneously the behaviour of each plane of small crystallites in terms of surface reconstruction, adsorption and catalytic activity. They are complementary to environmental transmission and scanning electron microscopies. [source]


    Synthesis of Nanotube Array Composed of an Amorphous Matrix Embedded with NaCl-Type SiC Crystallites by Chemical Vapor Infiltration Techniques

    JOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 6 2010
    Wen Yang
    Highly dense oriented arrays of nanotubes were synthesized via a chemical vapor infiltration process using anodic alumina membrane as a template. The nanotubes have a unique granular structure, which is composed of SiC nanocrystals embedded in an amorphous matrix. X-ray diffraction and high-resolution transmission electron microscopy examinations both indicate an NaCl-type crystalline structure of the SiC nanocrystals in the nanotubes. The process described here can be extended to the preparation of other nanomaterials that are suitable to be obtained via a vapor,solid approach. [source]


    NiZnCu Ferrite Thick Film with Nano Scale Crystallites Formed by the Aerosol Deposition Method

    JOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 9 2004
    Maxim Lebedev
    This paper describes the magnetic properties of NiZnCu ferrite film deposited at room temperature by an aerosol deposition method (ADM). The thickness of the film was 6 ,m and the deposition rate was estimated as 2 ,m/min. The microstructure of as-deposited at room temperature films consists of randomly oriented nanocrystallites with a size of 20 nm. As-deposited and annealed films exhibited the following magnetic properties: intensity of magnetization Ms= 0.147 T (117 emu/cm3), coercivity Hc= 40.58 kA/m (510 Oe); and Ms= 0.3 T (250 emu/cm3), Hc= 14.95 kA/m (188 Oe), respectively. [source]


    X-ray Diffraction Investigations of Microstructure of Calcium Hydroxide Crystallites in the Interfacial Transition Zone of Concrete

    JOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 12 2003
    Valeri S. Harutyunyan
    This work presents theoretical and experimental X-ray diffractometry investigations of the morphology and deformation state of calcium hydroxide (Ca(OH)2, CH) crystallites in the interfacial transition zone of concrete. Based on the developed theoretical approach, the distributions of CH crystallites and their coherent domains over strains and sizes are reconstructed. The average amounts of planar defects, cracks, and possible stacking faults within a CH crystallite are estimated. A comparative analysis is conducted for the morphology of CH texture depending on the type of aggregate particles (granite and smoky quartz) used. [source]


    Current-Voltage Characterisation of Monolayer-Supported Au-Nanoclusters by Scanning Tunnelling Microscopy under Ambient Conditions

    EUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 18 2005
    Volker Jacobsen
    Abstract The current-voltage characteristics of a double-tunnel junction based on a gold crystallite with a diameter of ca. 2 nm, separated from a gold surface by ca. 1 nm was investigated by scanning tunnelling microscopy. The sample architecture was built by attaching gold nanoparticles covered with 2-mercaptosuccinic acid to an atomically flat gold surface which was covered by a self-assembled monolayer (SAM) of 6-amino-1-hexanethiol. Surface plasmon and infrared spectroscopy as well as STM imaging were employed to identify suitable preparation conditions and prove the existence of the desired architecture. No reproducible steps in the current-voltage characteristics are observed on this system under ambient conditions. Nonetheless, a sound signature for tunnelling through the double-tunnel junction is established by a quantitative fit of the averaged experimental data to a theoretical model of a single-tunnel junction. Firstly, the current on the particle is strongly reduced at low absolute external voltage and secondly the current voltage characteristics are asymmetric. Since both deviations from theory are absent in reference experiments on the bare monolayer, they may serve as a robust signature for double-tunnel junctions and open the door to the investigation of single-electron tunnelling under ambient conditions. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2005) [source]


    The morphology and characterization of starch from Pueraria lobata (Willd.) Ohwi

    INTERNATIONAL JOURNAL OF FOOD SCIENCE & TECHNOLOGY, Issue 6 2002
    Xian-Feng Du
    Pueraria lobata (Willd.) Ohwi starch and its components were characterized. Scanning electron microscopy of the starch granules showed they were oval and polygonal in shape. Centric birefringence was clearly observed when viewed under polarized light. The gelatinization temperature range was 61,64,70.5 °C. The iodine affinity value (4.12%) indicated an amylose content of 21.68%. Brabender amylograms showed a fairly high maximum viscosity and very low breakdown, indicating high hot stability of the viscosity. The starch underwent a single-stage swelling power pattern over one temperature range, and the solubility pattern paralleled the swelling power. The X-ray diffraction pattern of the starch showed a Ca-type crystallite. The gel chromatogram of the starch demonstrated the polydispersity of its molecular weight distribution. [source]


    Effect of a crystallite size distribution on X-ray diffraction line profiles and whole-powder-pattern fitting

    JOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 3-2 2000
    J. I. Langford
    A distribution of crystallite size reduces the width of a powder diffraction line profile, relative to that for a single crystallite, and lengthens its tails. It is shown that estimates of size from the integral breadth or Fourier methods differ from the arithmetic mean of the distribution by an amount which depends on its dispersion. It is also shown that the form of `size' line profiles for a unimodal distribution is generally not Lorentzian. A powder pattern can be simulated for a given distribution of sizes, if it is assumed that on average the crystallites have a regular shape, and this can then be compared with experimental data to give refined parameters defining the distribution. Unlike `traditional' methods of line-profile analysis, this entirely physical approach can be applied to powder patterns with severe overlap of reflections, as is demonstrated by using data for nanocrystalline ceria. The procedure is compared with alternative powder-pattern fitting methods, by using pseudo-Voigt and Pearson VII functions to model individual line profiles, and with transmission electron microscopy (TEM) data. [source]


    Synthesis and crystallization behavior of acetal copolymer/silica nanocomposite by in situ cationic ring-opening copolymerization of trioxane and 1,3-dioxolane

    JOURNAL OF APPLIED POLYMER SCIENCE, Issue 3 2008
    Lanhui Sun
    Abstract The acetal copolymer/silica nanocomposite was prepared by in situ bulk cationic copolymerization of trioxane and 1,3-dioxolane in the presence of nanosilica. The crystallization behavior of acetal copolymer/silica nanocomposite was studied by AFM, DSC, XRD, and CPOM, and the macromolecular structure of acetal copolymer/silica nanocomposite was characterized by FTIR and 1H-NMR. The 1H-NMR results showed that the macromolecular chain of acetal copolymer had more than two consecutive 1,3-dioxolane units in an oxymethylene main chain, while that of acetal copolymer/silica nanocomposite had only one 1,3-dioxolane unit in an oxymethylene main chain. There existed interaction between the macromolecular chains and nanoparticles (such as hydrogen bonds and coordination). On one hand, nanoparticles acted as nucleation center, which accelerated the crystallization rate but reduced the crystallinity. The spherulite sizes also decreased with addition of nanoparticles attributed to the nucleation effect. On the other hand, the presence of nanoparticles interrupted the spherical symmetry of the crystallite. In conclusion, the high surface energy and small scale of nanoparticles have a prominent impact on the polymerization mechanism and crystallization behavior of nanocomposite. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008 [source]


    Use of a hexapod in diffraction measurements of substrate-supported crystals of organic semiconductors

    JOURNAL OF SYNCHROTRON RADIATION, Issue 6 2009
    Lin Yang
    Thin films of organic semiconductor prepared on substrates generally contain crystals that have one common crystal plane parallel to the substrate but random in-plane orientations. In diffraction measurements of these structures, it is often required to anchor the X-ray beam on a fixed spot on the sample, such as an optically visible crystallite or island. Here, a hexapod is used in place of a traditional multi-circle diffractometer to perform area-detector-based diffraction measurements on an actual device that contains 6,13-bis(triisopropylsilyethynyl)-pentacene (TIPS-pentacene) crystals. The hexapod allows for sample rotations about any user-defined rotation center. Two types of complex sample motions have been programmed to characterize the structure of the TIPS-pentacene crystal: an in-plane powder average has been performed at a fixed grazing-incident angle to determine the lattice parameters of the crystal; then the in-plane component of the scattering vector was continuously rotated in transmission geometry to determine the local crystal orientation. [source]


    X-ray Diffraction Investigations of Microstructure of Calcium Hydroxide Crystallites in the Interfacial Transition Zone of Concrete

    JOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 12 2003
    Valeri S. Harutyunyan
    This work presents theoretical and experimental X-ray diffractometry investigations of the morphology and deformation state of calcium hydroxide (Ca(OH)2, CH) crystallites in the interfacial transition zone of concrete. Based on the developed theoretical approach, the distributions of CH crystallites and their coherent domains over strains and sizes are reconstructed. The average amounts of planar defects, cracks, and possible stacking faults within a CH crystallite are estimated. A comparative analysis is conducted for the morphology of CH texture depending on the type of aggregate particles (granite and smoky quartz) used. [source]


    Crystallite and Grain-Size-Dependent Phase Transformations in Yttria-Doped Zirconia

    JOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 2 2003
    Arun Suresh
    In pure zirconia, ultrafine powders are often observed to take on the high-temperature tetragonal phase instead of the "equilibrium" monoclinic phase. The present experiments and analysis show that this observation is one manifestation of a much more general phenomenon in which phase transformation temperatures shift with crystallite/grain size. In the present study, the effect of crystallite (for powders) and grain (for solids) size on the tetragonal , monoclinic phase transformation is examined more broadly across the yttria,zirconia system. Using dilatometry and high-temperature differential scanning calorimetry on zirconia samples with varying crystallite/grain sizes and yttria content, we are able to show that the tetragonal , monoclinic phase transformation temperature varies linearly with inverse crystallite/grain size. This experimental behavior is consistent with thermodynamic predictions that incorporate a surface energy difference term in the calculation of free-energy equilibrium between two phases. [source]


    Synthesis of Conducting Polymer Spiral Nanostructures Using a Surfactant Crystallite Template

    MACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 11 2009
    Yong Wang
    Abstract The present work describes, for the first time, the synthesis of spiral nanostructures of conducting polymers by chemical oxidant polymerization using a hydrated surfactant (sodium dodecyl sulfonate (SDSn)) crystallite template. A spiral dislocation structure on the surface of a hydrated SDSn crystallite has been observed and is responsible for the growth of the spiral nanoarchitecture of conducting polymers (polypyrrole, polyaniline). Ammonium peroxydisulfate (APS) has a strong tendency to induce the formation of a spiral dislocation structure of hydrated SDSn crystallites. The mechanism of adsorption of pyrrole or aniline oligomers on the steps of dislocation is proposed for the growth of conducting polymer spirals. [source]


    Growth behavior and microstructure of ZnO epilayer on ,-LiAlO2(100) substrate by chemical vapor deposition

    PHYSICA STATUS SOLIDI (A) APPLICATIONS AND MATERIALS SCIENCE, Issue 2 2009
    Liuwen Chang
    Abstract Low lattice-mismatched ,-LiAlO2(100) substrates were employed to grow ZnO epitaxial films by chemical vapor deposition. The influence of growth temperature on growth behavior of ZnO was investigated. Results indicated that the low lattice-matched (100) crystallites nucleate on substrate at all growth temperatures employed. However, a second type of crystallites having an (0001) orientation can also nucleate on substrate at low growth temperature of 575 °C and 640 °C. The growth rate of the later crystallite is, however, higher than that of the (100) one and finally results in a single crystalline ZnO film having an [0001] azimuthal orientation. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source]


    Synthesis of ZnO whiskers with different aspect ratios by a facile solution route

    PHYSICA STATUS SOLIDI (A) APPLICATIONS AND MATERIALS SCIENCE, Issue 7 2008
    Juan Xie
    Abstract Monodispersed zinc oxide (ZnO) whiskers with different aspect ratios were successfully prepared via a simple solution route at low temperature. It is found that the diameter and aspect ratio of ZnO whiskers depend critically on the structure and type of ionic surfactant added in the reaction solution. To further understand the effect of the surfactants on the formation process of ZnO whiskers, concentration measurements of Zn(II) remaining in the solution as well as scanning electron microscopy (SEM) and X-ray powder diffraction (XRD) analyses of the solid product have been made at regular intervals throughout the reaction with and without the surfactants. A possible formation process has been reasonably suggested based on these systematic experimental results. It is believed that anion surfactants are capable of slowing down the nucleation and growth rate of ZnO crystallite, which is favorable for the anisotropic growth habit of ZnO crystal to form needle-like whiskers. (© 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source]


    Hopping parameters in densely packed submicron crystallites

    PHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 3 2008
    L. J. Huijbregts
    Abstract The density of states g (E) in the hopping process in closely packed crystallites is expected to differ from g (E) within a single crystallite [Zhang and Shklovskii, Phys. Rev. B 70, 115317 (2004)]. Dielectric scans are well suited to quantify these differences. Here we illustrate the method by discussing the results on Phthalcon-11, a cobalt phthalocyanine with submicron dimensions. (© 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source]


    Spatial orientation of nanoclay and crystallite in microcellular injection molded polyamide-6 nanocomposites

    POLYMER ENGINEERING & SCIENCE, Issue 6 2007
    Mingjun Yuan
    Three different types of characteristic structures-microcells, nanoclay, and crystallite lamella-exist in injection molded polyamide-6 microcellular nanocomposites. These structures are in completely different scales. The spatial orientation of these microscale structures crucially determines the material's bulk properties. Based on scanning electron microscopy, transmission electron microscopy, and two-dimensional X-ray diffractometry measurements, it was found that the nanoclay and the crystallite formed special geometric structures around the microcells and near the part skins. The nanoclay platelets lay almost parallel to the surfaces of the molded parts. Preferred orientation of the crystallites was induced by the presence of the nanoclay. A molecular-based model is proposed to describe the structural hierarchy and correlations among the microcells, nanoclay, and crystallite lamella. From the small-angle X-ray scattering experiments, it was found that microcellular injection molding produces relatively smaller crystallite lamella than that of conventional injection molding, and that for both solid and microcellular neat resin parts the crystallite lamella thickness at the part skin is smaller than that at the core. Polarized optical microscopy results also indicated that the size of crystallites in the microcellular neat resin and nanocomposite parts is smaller than that in the corresponding solid parts. POLYM. ENG. SCI., 47:765,779, 2007. © 2007 Society of Plastics Engineers [source]


    `Segmented' crystals solved using synchrotron radiation: (2S,3R,4S,5R)-4-(10,10-dimethyl-3,3-dioxo-3,6 -thia-4-azatricyclo[5.2.1.01,5]decan-4-ylcarbonyl)-2,6-diphenylperhydropyrrolo[3,4- c]pyrrole-1,3-dione

    ACTA CRYSTALLOGRAPHICA SECTION C, Issue 7 2009
    Graeme J. Gainsford
    The title compound, C29H31N3O5S, forms needle-shaped `segmented' crystals, thereby inhibiting successful single-crystal data collection using conventional laboratory facilities. One crystallite of dimensions 0.15 × 0.03 × 0.01,mm yielded sufficent single-crystal diffraction data on the Australian Synchrotron PX1 beamline. The two independent molecules in the asymmetric unit are nearly superimposable and show only minor conformational deviations from closely related compounds. The molecules pack using one N,H...O hydrogen bond and several phenyl C,H...O(=S), phenyl C,H...O(=C) and methylene C,H...O(=C) hydrogen bonds and weak C,H..., interactions. [source]


    Synthesis and morphology of nanosized zeolite L

    CRYSTAL RESEARCH AND TECHNOLOGY, Issue 2 2010
    S. Sadegh Hassani
    Abstract AFM is a powerful tool for imaging nanoscale surface features; it provides two and three dimensional crystal structure images and other information about actual surface of zeolite crystallites. In this paper, nanosized zeolite L is synthesized in different crystallization times and a study of crystal growth of zeolite L is reported using atomic force microscopy (AFM). X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) techniques are used for characterization of the as synthesized samples. TEM and two-dimensional AFM images indicate that the zeolite particles are in a nano-range and they have hexagonal structure. (© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source]


    Influence of the atmosphere on the growth of LiYF4 single crystal fibers by the micro-pulling-down method

    CRYSTAL RESEARCH AND TECHNOLOGY, Issue 2 2009
    D. Maier
    Abstract Micro-pulling-down growth of LiYF4 single crystal fibers have been performed under different gas atmospheres using stoichiometric LiYF4 single crystal pieces from prior Czochralski experiments as starting material. Completely transparent and phase pure LiYF4 single crystal fibers could be obtained after evacuation of the recipient to 2×10 -6 mbar and subsequent filling with pure (99.995%) CF4 gas. Using a gas mixture of 5% CF4 in Argon or pure 5N Argon leads to the formation of micro crystallites of oxofluorides on the surface. Evacuating only to 3 × 10 -3 mbar leads, independently of atmosphere, to completely white fibers that are heavily contaminated with oxofluorides. DSC measurements of the completely transparent fiber grown under pure CF4 atmosphere reveal congruent melting behavior. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source]


    Growth and characterization of Nd, Yb , yttrium oxide nanopowders obtained by sol-gel method

    CRYSTAL RESEARCH AND TECHNOLOGY, Issue 12 2007
    A. Rzepka
    Abstract Nanopowders of Y2O3 pure, doped and codoped by Nd3+, Yb3+ were obtained by sol-gel method. Solution with ethylene glycol was choosed as the proper solution where crystallites of powder with Nd and Yb dopants had the same size. Finally the one-phased compounds of Y2O3 doped 0.5 at% Nd and 1, 2 or 4 at% Yb were obtained. Grain growth and their morphology were investigated in various temperature and time of heating. The changes of crystallite sizes and lattice constants in relation to the heating time and temperature for the composition Y2O3 doped 0.5 at% Nd and 2 at% Yb are presented. Y2O3 containing 0,5 at% of Nd exhibits intense luminescence bands centered at 920 nm, 1100 nm and 1360 nm whereas a single band at about 1020 nm appears in samples co-doped with neodymium and ytterbium. Luminescence spectra recorded did not depend on the sample preparation procedure and size of grains. OH impurity affects critically the relaxation dynamics of luminescent ion in nanopowders. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source]


    Raman spectroscopic and X-ray investigation of stressed states in diamond-like carbon films

    CRYSTAL RESEARCH AND TECHNOLOGY, Issue 1-2 2005
    R. Krawietz
    Abstract The non-destructive characterization of intrinsic stress is very important to evaluate the reliability of devices based on diamond-like carbon (DLC) films. Whereas the only requirement for the X-ray diffraction method is a crystalline state of specimen, Raman spectroscopic stress analysis is restricted to materials showing intensive and sharp Raman peaks. On the other hand, Raman spectroscopy offers the possibility to measure stress profiles with lateral resolution of about 1 micron. The results of stress measurements in DLC films using both X-ray diffraction and Raman spectroscopy are found in very good correspondence. Mean stress in carbon films consisting of very small crystallites on silicon substrates has been determined by measuring and fitting the stress profiles in the substrate near artificial vertical film edges. (© 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source]


    Inter-crystallite nanoretention of self-etching adhesives at enamel imaged by transmission electron microscopy

    EUROPEAN JOURNAL OF ORAL SCIENCES, Issue 6 2002
    Matthias Hannig
    The purpose of this in vitro study was to analyse the mode of action of self-etching adhesive systems when applied for resin-to-enamel bonding. Transmission electron microscopy was used to investigate the enamel,resin interface after application of non-rinsing self-etching adhesive systems based on phosphoric acid estered methacrylates (Clearfil Liner Bond 2, Clearfil SE Bond, Etch & Prime 3.0 and Resulcin AquaPrime) compared with conventional phosphoric acid etching and bonding (Heliobond). Non-decalcified ultrathin sections from the interface between enamel and self-etching adhesive systems revealed a 1.5,3.2-µm deep enamel surface layer characterized by a less-dense arrangement of enamel crystallites separated from each other by nanometer-sized spaces. A 1.5,3.2-µm wide, netlike resinous structure was observed in corresponding decalcified specimens, indicating that self-etching priming agents dissolve the peripheral and central part of the enamel crystallites, while simultaneously promoting inter- and intra-crystallite monomer infiltration. A similar pattern, but greater depth (6.9 µm) of enamel surface hybridization was found in the phosphoric acid-etched and bonded specimens. The nanoretentive interlocking between enamel crystallites and resin could explain the potential of self-etching adhesive systems in resin-to-enamel bonding despite the less distinct enamel etching pattern observed in scanning electron microscopy investigations. [source]


    Hydroxyapatite/Bioactive Glass Films Produced by a Sol,Gel Method: In Vitro Behavior

    ADVANCED ENGINEERING MATERIALS, Issue 11 2009
    Nihat C. Köseo
    Abstract Hydroxyapatite (HA) and HA/bioactive glass (49S) films were deposited on Si(100) substrates by a sol,gel dip-coating method. The microstructure and in vitro bioactivity of the films were investigated by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS). Polycrystalline HA and amorphous bioactive glass films were obtained after annealing at 600 and 400,°C, respectively. The crystallization temperature of HA was determined to be around 568,°C. The surfaces of the HA films were covered with an apatite layer consists of spherulites formed by nanosized needle-like aggregates after the soaking in simulated body fluid (SBF) for 10 days, while amorphous HA/bioactive glass surface was covered with larger spherical crystallites. Both XPS and EDS results obtained from HA/bioactive glass film, after soaking in SBF, showed increasing P amounts on the surface at the expense of Si. The higher density of the newly formed layer on HA/bioactive glass surface than that of the HA surface after 10 days of soaking was evidence of increased reaction rate and apatite forming ability when bioactive glass layer is present on the HA films. [source]


    In Situ Observation of Dynamic Recrystallization in the Bulk of Zirconium Alloy (Adv. Eng.

    ADVANCED ENGINEERING MATERIALS, Issue 8 2009
    Mater.
    The cover shows the in-situ diffraction setup. A fine synchrotron beam transmits the sample situated in a (heated) load frame and scatters into Debye-Scherrer cones. Large crystallites map onto spots onto the 2D detector rather than continuous rings. In the background, the intensity distribution of one selected reflection - here beta-Zr 110 - is plotted in color scale as a function of azimuthal angle (horizontal axis) and time (vertical axis) revealing the different states during thermo-mechanical processing. More details can be found in the article by K.-D. Liss on page 637. [source]


    Abrupt Morphology Change upon Thermal Annealing in Poly(3-Hexylthiophene)/Soluble Fullerene Blend Films for Polymer Solar Cells

    ADVANCED FUNCTIONAL MATERIALS, Issue 5 2010
    Minjung Shin
    Abstract The in situ morphology change upon thermal annealing in bulk heterojunction blend films of regioregular poly(3-hexylthiophene) (P3HT) and 1-(3-methoxycarbonyl)-propyl-1-phenyl-(6,6)C61 (PCBM) is measured by a grazing incidence X-ray diffraction (GIXD) method using a synchrotron radiation source. The results show that the film morphology,including the size and population of P3HT crystallites,abruptly changes at 140,°C between 5 and 30,min and is then stable up to 120,min. This trend is almost in good agreement with the performance change of polymer solar cells fabricated under the same conditions. The certain morphology change after 5,min annealing at 140,°C is assigned to the on-going thermal transition of P3HT molecules in the presence of PCBM transition. Field-emission scanning electron microscopy measurements show that the crack-like surface of blend films becomes smaller after a very short annealing time, but does not change further with increasing annealing time. These findings indicate that the stability of P3HT:PCBM solar cells cannot be secured by short-time annealing owing to the unsettled morphology, even though the resulting efficiency is high. [source]


    Enhanced Thermal Stability and Efficiency of Polymer Bulk-Heterojunction Solar Cells by Low-Temperature Drying of the Active Layer

    ADVANCED FUNCTIONAL MATERIALS, Issue 5 2010
    Ching Lin
    Abstract This study addresses two key issues, stability and efficiency, of polymer solar cells based on blended poly(3-hexylthiophene) (P3HT) and [6,6]-phenyl-C61-butyric acid methyl ester (PCBM) by demonstrating a film-forming process that involves low-temperature drying (,5,°C) and subsequent annealing of the active layer. The low-temperature process achieves 4.70% power conversion efficiency (PCE) and ,1250,h storage half-life at 65,°C, which are significant improvements over the 3.39% PCE and ,143,h half-life of the regular room-temperature process. The improvements are attributed to the enhanced nucleation of P3HT crystallites as well as the minimized separation of the P3HT and PCBM phases at the low drying temperature, which upon post-drying annealing results in a morphology consisting of small PCBM-rich domains interspersed within a densely interconnected P3HT crystal network. This morphology provides ample bulk-heterojunction area for charge generation while allowing for facile charge transport; moreover, the P3HT crystal network serves as an immobile frame at heating temperatures less than the melting point (Tm) of P3HT, thus preventing PCBM/P3HT phase separation and the corresponding device degradation. [source]


    Novel Magnetic Hydroxyapatite Nanoparticles as Non-Viral Vectors for the Glial Cell Line-Derived Neurotrophic Factor Gene

    ADVANCED FUNCTIONAL MATERIALS, Issue 1 2010
    Hsi-Chin Wu
    Abstract Nanoparticles (NPs) of synthetic hydroxyapatite (Hap) and natural bone mineral (NBM) are rendered magnetic by treatment with iron ions using a wet-chemical process. The magnetic NPs (mNPs), which are about 300,nm in diameter, display superparamagnetic properties in a superconducting quantum interference device, with a saturation magnetization of about 30,emu g,1. X-ray diffraction and transmission electron microscopy reveal that the magnetic properties of the NPs are the result of the hetero-epitaxial growth of magnetite on the Hap and NBM crystallites. The mNPs display a high binding affinity for plasmid DNA in contrast to magnetite NPs which do not bind the plasmid well. The mHap and mNBM NPs result in substantial increases in the transfection of rat marrow-derived mesenchymal stem cells with the gene for glial cell line-derived neurotrophic factor (GDNF), with magnetofection compared to transfection in the absence of a magnet. The amount of GDNF recovered in the medium approaches therapeutic levels despite the small amount of plasmid delivered by the NPs. [source]


    High-Pressure Synthesis of Tantalum Nitride Having Orthorhombic U2S3 Structure

    ADVANCED FUNCTIONAL MATERIALS, Issue 14 2009
    Andreas Zerr
    Abstract Among binary compounds, there is a high potential for discovery of novel members (polymorphic phases or compounds) of the nitrides of transition metals group due to a pronounced dependence of the oxidation state of the metals (M) on pressure. The power of high pressure,high temperature (HP-HT) route for synthesis of binary nitrides has already been demonstrated by the discovery of cubic nitrides of the group 4 and 14 elements, of crystalline polymorphs of P3N5, and by reports on formation of four noble metal nitrides. It is anticipated that such HP products exhibit, in addition to enhanced elastic and mechanical behavior, other functional properties making them interesting for industrial applications. Here, HP,HT synthesis research is extended to nitrides of group 5 elements, resulting in the discovery of a novel hard tantalum nitride, exhibiting U2S3 structure: , -Ta2N3 (Pbnm, a,=,8.1911(17),Å, b,=,8.1830(17),Å, c,=,2.9823(3),Å). The stoichiometry is supported by two independent means, verifying that , -Ta2N3 is the first thermodynamically stable transition metal nitride with a N:M ratio exceeding 4:3. Due to its high hardness and peculiar texture (needle-like and granular crystallites), , -Ta2N3 may find practical applications as a hard fracture resistant material. [source]


    A Spring-Like Behavior of Chiral Block Copolymer with Helical Nanostructure Driven by Crystallization

    ADVANCED FUNCTIONAL MATERIALS, Issue 3 2009
    Yeo-Wan Chiang
    Abstract The crystallization of helical nanostructure resulting from the self-assembly of a chiral diblock copolymer, poly(styrene)- b -poly(L -lactide) (PS-PLLA), is studied. Various crystalline PS-PLLA nanostructures are obtained by controlling the crystallization temperature of PLLA (Tc,PLLA), at which crystalline helices and crystalline cylinders occur while Tc,PLLA,<,Tg,PS (the glass transition temperature of PS) and Tc,PLLA,,,Tg,PS, respectively. As evidenced by selected-area electron diffraction and two-dimensional X-ray diffraction results, the PLLA crystallites under confinement reveal a unique anisotropic character regardless of the crystallization temperature. On the basis of observed uniaxial scattering results the PLLA crystallites grown within the microdomains are identified as crystals with preferential growth directions either along the [100] or along the [110]-axes of the PLLA crystalline unit cell, at which the molecular chains and the growth direction are normal and parallel to the central axes of helices, respectively. The formation of this exclusive crystalline growth is attributed to the spatial confinement effect for crystallization. While Tc,PLLA,<,Tg,PS, owing to the directed crystallization by helical confinement, the preferential crystalline growth leads to the crystallization following a helical track with growth direction parallel to the central axes of helices through a twisting mechanism. Consequently, winding crystals with specific crystallographic orientation within the helical microdomains can be found. By contrast, while Tc,PLLA,,,Tg,PS, the preferential growth may modulate the curvature of microdomains by shifting the molecular chains to access the fast path for crystalline growth due to the increase in chain mobility. As a result, a spring-like behavior of the helical nanostructure can be driven by crystallization so as to dictate the transformation of helices, resulting in crystalline cylinders that might be applicable to the design of switchable large-strain actuators. [source]