Grazing-incidence Small-angle X-ray Scattering (grazing-incidence + small-angle_x-ray_scattering)

Distribution by Scientific Domains

Selected Abstracts

Electropolymerization of a Bifunctional Ionic Liquid Monomer Yields an Electroactive Liquid-Crystalline Polymer

Sungwon Lee
Abstract The preparation and polymerization of a bifunctional imidazolium-based ionic liquid (IL) monomer that incorporates both a vinyl group and a thiophene moiety is reported. Potentiodynamic electropolymerization of the monomer produces an optically birefringent polymer film that strongly adheres to the electrode surface. Fourier transform IR spectroscopy shows that polymerization occurs through both the vinyl and thienyl groups. Cylic voltammetry (CV) is used to determine the polymer oxidation potential (1.66,V) and electrochemical bandgap, Eg, of 2.45,eV. The polymer exhibits electrochromism, converting from yellow in the neutral form (,max,=,380,nm) to blue in the polaronic state at 0.6,V (,max,=,672,nm) and to blue-grey in the bipolaronic state at 1.2,V (,max,>,800,nm). Topographic atomic force microscopy (AFM) images reveal isolated (separated) fibrils. Grazing-incidence small-angle X-ray scattering (GISAXS) studies indicate a lamellar structure with a lattice spacing of 3.2,nm. Wide-angle X-ray diffraction (WAXD) studies further suggest that the polymerized thiophene sheets are oriented perpendicular to the polymerized vinylimidazolium. The electrical conductivity, as determined by four-probe dc conductivity measurements was found to be 0.53,S cm,1 in the neutral form and 2.36,S cm,1 in the iodine-doped state, values higher than typically observed for polyalkylthiophenes. The structural ordering is believed to contribute to the observed enhancement of the electrical conductivity. [source]

Photophysics and Photocurrent Generation in Polythiophene/Polyfluorene Copolymer Blends

Christopher R. McNeill
Abstract Here, studies on the evolution of photophysics and device performance with annealing of blends of poly(3-hexylthiophene) with the two polyfluorene copolymers poly((9,9-dioctylfluorene)-2,7-diyl-alt-[4,7-bis(3-hexylthien-5-yl)-2,1,3-benzothiadiazole]-2,,2,,-diyl) (F8TBT) and poly(9,9-dioctylfluorene-co-benzothiadiazole) (F8BT) are reported. In blends with F8TBT, P3HT is found to reorganize at low annealing temperatures (100,C or below), evidenced by a redshift of both absorption and photoluminescence (PL), and by a decrease in PL lifetime. Annealing to 140,C, however, is found to optimize device performance, accompanied by an increase in PL efficiency and lifetime. Grazing-incidence small-angle X-ray scattering is also performed to study the evolution in film nanomorphology with annealing, with the 140,C-annealed film showing enhanced phase separation. It is concluded that reorganization of P3HT alone is not sufficient to optimize device performance but must also be accompanied by a coarsening of the morphology to promote charge separation. The shape of the photocurrent action spectra of P3HT:F8TBT devices is also studied, aided by optical modeling of the absorption spectrum of the blend in a device structure. Changes in the shape of the photocurrent action spectra with annealing are observed, and these are attributed to changes in the relative contribution of each polymer to photocurrent as morphology and polymer conformation evolve. In particular, in as-spun films from xylene, photocurrent is preferentially generated from ordered P3HT segments attributed to the increased charge separation efficiency in ordered P3HT compared to disordered P3HT. For optimized devices, photocurrent is efficiently generated from both P3HT and F8TBT. In contrast to blends with F8TBT, P3HT is only found to reorganize in blends with F8BT at annealing temperatures of over 200,C. The low efficiency of the P3HT:F8BT system can then be attributed to poor charge generation and separation efficiencies that result from the failure of P3HT to reorganize. [source]

Self-Assembly of Nanoparticle,Copolymer Mixtures: A Kinetic Point of View,

J. He
The prediction of synergistic effects between two self-organizing systems is tested. In,situ grazing-incidence small-angle X-ray scattering (see figure) is used during thermal annealing of a nanoparticle,copolymer mixture, and shows that the orientation of the microdomains begins at the free surface and propagates in the film towards the substrate. This synergistic interaction is shown to apply to both cylindrical and lamellar block-copolymer morphologies. [source]

Structure of PbTe(SiO2)/SiO2 multilayers deposited on Si(111)

Guinther Kellermann
The structure of thin films composed of a multilayer of PbTe nanocrystals embedded in SiO2, named as PbTe(SiO2), between homogeneous layers of amorphous SiO2 deposited on a single-crystal Si(111) substrate was studied by grazing-incidence small-angle X-ray scattering (GISAXS) as a function of PbTe content. PbTe(SiO2)/SiO2 multilayers were produced by alternately applying plasma-enhanced chemical vapour deposition and pulsed laser deposition techniques. From the analysis of the experimental GISAXS patterns, the average radius and radius dispersion of PbTe nanocrystals were determined. With increasing deposition dose the size of the PbTe nanocrystals progressively increases while their number density decreases. Analysis of the GISAXS intensity profiles along the normal to the sample surface allowed the determination of the period parameter of the layers and a structure parameter that characterizes the disorder in the distances between PbTe layers. [source]

GISAXS and protein nanotemplate crystallization: methods and instrumentation

Eugenia Pechkova
Microbeam grazing-incidence small-angle X-ray scattering (GISAXS) has been used and the technique has been improved in order to investigate protein nucleation and crystal growth, assisted by a protein nanotemplate. The aim is to understand the protein nanotemplate method in detail, as this method has been proved capable of accelerating and increasing crystal size and quality as well as inducing crystallization of proteins that are not crystallizable by classical methods. The nanotemplate experimental setup was used for drops containing growing lysozyme crystals at three different stages of growth. [source]

Depth profiling of polymer films with grazing-incidence small-angle X-ray scattering

Marsha A. Singh
A model-free method of reconstructing depth-specific lateral scattering from incident-angle-resolved grazing-incidence small-angle X-ray scattering (GISAXS) data is proposed. The information on the material which is available through variation of the X-ray penetration depth with incident angle is accessed through reference to the reflected branch of the GISAXS process. Reconstruction of the scattering from lateral density fluctuations is achieved by solving the resulting Fredholm integral equation with minimal a priori information about the experimental system. Results from simulated data generated for hypothetical multilayer polymer systems with constant absorption coefficient are used to verify that the method can be applied to cases with large X-ray penetration depths, as typically seen with polymer materials. Experimental tests on a spin-coated thick film of a blend of diblock copolymers demonstrate that the approach is capable of reconstruction of the scattering from a multilayer structure with the identification of lateral scattering profiles as a function of sample depth. [source]