INVESTIGATION OF C-60 SINGLE-CRYSTAL BY X-RAY-METHODS

C-60 Single crystals grown by a single-temperature-gradient technique were characterized by synchrotron radiation white beam x-ray topography and x-ray double crystal diffraction with Cu K-alpha 1 radiation on conventional x-ray source. The results show that the crystal is rather well crystallized, The x-ray topographies give an evidence of dendritic growth mechanism of C-60 Single crystal, and x-ray double crystal diffraction rocking curve shows that there are mosaic structural defects in the sample. A phase transition st 249+/-1.5% K from a simple cubic to a face centered cubic structure is confirmed by in situ observation of synchrotron radiation white beam x-ray topography with the temperature varing from 230 to 295 K.

Structural evolution of tensile deformed high-density polyethylene at elevated temperatures: Scanning synchrotron small- and wide-angle X-ray scattering studies

The structural evolution of an ice-quenched high-density polyethylene (HDPE) subjected to uniaxial tensile deformation at elevated temperatures was examined as a function of the imposed strains by means of combined synchrotron small-angle X-ray scattering (SAXS) and wide-angle X-ray scattering (WAXS) techniques. The data show that when stretching an isotropic sample with the spherulitic structure, intralamellar slipping of crystalline blocks was activated at small deformations, followed by a stress-induced fragmentation and recrystallization process yielding lamellar crystallites with their normal parallel to the stretching direction. Stretching of an isothermally crystallized HDPE sample at 120 degrees C exhibited changes of the SAXS diagram with strain similar to that observed for quenched HDPE elongated at room temperature, implying that the thermal stability of the crystal blocks composing the lamellae is only dependent on the crystallization temperature.

Uniaxial deformation of overstretched polyethylene: In-situ synchrotron small angle X-ray scattering study

Synchrotron small angle X-ray scattering was used to study the deformation mechanism of high-density polyethylene that was stretched beyond the natural draw ratio. New insight into the cooperative deformational behavior being mediated via slippage of micro-fibrils was gained. The scattering data confirm on the one hand the model proposed by Peterlin on the static structure of oriented polyethylene being composed of oriented fibrils, which are built by bundles of micro-fibrils. On the other hand it was found that deformation is mediated by the slippage of the micro-fibrils and not the slippage of the fibrils. In the micro-fibrils, the polymer chains are highly oriented both in the crystalline and in the amorphous regions. When stretching beyond the natural draw ratio mainly slippage of micro-fibrils past each other takes place. The thickness of the interlamellar amorphous layers increases only slightly. The coupling force between micro-fibrils increases during stretching due to inter-microfibrillar polymer segments being stretched taut thus increasingly impeding further sliding of the micro-fibrils leading finally to slippage of the fibrils.

Structural evolution of tensile-deformed high-density polyethylene during annealing: Scanning synchrotron small-angle X-ray scattering study

The structural evolution of high-density polyethylene subjected to uniaxial tensile deformation was investigated as a function of strain and after annealing at different temperatures using a scanning synchrotron small-angle X-ray scattering (SAXS) technique. The results confirm that in the course of tensile deformation intralamellar block slips were activated at small deformations followed by a stress-induced fragmentation and recrystallization process yielding thinner lamellae with their normal parallel to the stretching direction. The original sheared lamellae underwent severe internal deformation so that they were even less stable than the newly developed thinner lamellae. Accordingly, annealing results in a melting of the original crystallites even at moderate strains where the stress-induced fragmentation and recrystallization just sets in and generates a distinctly different form of lamellar stacks aligned along the drawing direction. It was found that the lamellae newly formed during stretching at moderate strains remain stable at lower temperature. Only at a very high annealing temperature of 120 degrees C can they be melted, leading to an isotropic distribution of the lamellar structure.

Non-affine structural evolution of soft colloidal crystalline latex films under stretching as observed via synchrotron X-ray scattering

A polymer dispersion consisting of soft latex spheres with a diameter of 135 nm was used to produce a crystalline film with face-centered cubic (fcc) packing of the spheres. Different from conventional small-molecule and hardsphere colloidal crystals, the crystalline latex film in the present case is soft (i.e., easily deformable). The structural evolution of this soft colloidal latex film under stretching was investigated by in-situ synchrotron ultra-small-angle X-ray scattering. The film exhibits polycrystalline scattering behavior corresponding to fcc structure. Stretching results not only in a large deformation of the crystallographic structure but also in considerable nonaffine deformation at high draw ratios. The unexpected nonaffine deformation was attributed to slippage between rows of particles and crystalline grain boundaries. The crystalline structure remains intact even at high deformation, suggesting that directional anisotropic colloidal crystallites can be easily produced.

In situ study of nanostructure and morphological development during the crystal-mesophase transition of poly(di-n-hexylsilane) and poly(di-n-butylsilane) by X-ray and hot-stage AFM

Nanostructure and morphology and their development of poly(di-n-hexylsilane) (PDHS) and poly(di-n-butylsilane) (PDBS) during the crystal-mesophase transition are investigated using small angle X-ray scattering (SAXS), wide angle X-ray diffraction and hot-stage atomic force microscopy. At room temperature, PDHS consists of stacks of lamellae separated by mesophase layers, which can be well accounted using an ideal two-phase model. During the crystal-mesophase transition, obvious morphological changes are observed due to the marked changes in main chain conformation and intermolecular distances between crystalline phase and mesophase. In contrast to PDHS, the lamellae in PDBS barely show anisotropy in dimensions at room temperature. The nonperiodic structure and rather small electronic density fluctuation in PDBS lead to the much weak SAXS. The nonperiodic structure is preserved during the crystal-mesophase transition because of the similarity of main chain conformation and intermolecular distances between crystalline phase and mesophase.

High-temperature X-ray diffraction studies on polyamide6/clay nanocomposites upon annealing

The influence of nanodispersed clay on the alpha crystalline structure of polyamide 6 (PA6) was examined in-situ with X-ray diffraction (XRD) between room temperature and melting. In pure PA6 upon annealing the alpha crystalline phase was substituted by an unstable pseudohexagonal phase at 150degreesC, then it transformed into a new stable crystalline structure - high temperature alpha' phase above the transition temperature. However, in PA6/clay nanocomposite (PA6CN), the alpha phase did not present crystalline phase transition on heating. The increase in the annealing temperature only led to continuous intensity variation. The different behaviors were caused by the confined spaces formed by silicate layers, which constrained the mobility of the polymer chains in-between.

1,1 '-di(tert-butyl)metallocenium cations. The x-ray crystal structures of [M((C5H4Bu)-Bu-t)(2)]PF6 (M = Fe, Co) and [Co((C5H4Bu)-Bu-t)(2)](2)CoCl4

The hexafluorophosphate salts [Fe((C5H4Bu)-Bu-t)(2)]PF6 (1) and [Co((C5H4Bu)-Bu-t)(2)]PF6 (2) crystallize in isotypic structures with centrosymmetric cations which have a staggered (transoid) conformation of the exactly parallel ring Ligands (conformational angle tau = 180 degrees). The tetrachlorocobaltate salt, [CO((C5H4Bu)-Bu-t)(2)](2)CoCl4 (3), contains one almost eclipsed (tau = 140.4 degrees) and one almost staggered (tau = 101.4 degrees) cobaltocenium cation; in both cases, the cyclopentadienyl ring planes are slightly inclined (by alpha = 5.4 degrees and 4.1 degrees, respectively) to give more room to the tert-butyl substituents which are bent away from the metal in all three complexes 1 - 3.

Local similarity in organic crystals and the non-uniqueness of X-ray powder patterns

Two new concepts for molecular solids, 'local similarity' and 'boundary-preserving isometry', are defined mathematically and a theorem which relates these concepts is formulated. 'Locally similar' solids possess an identical short-range structure and a 'boundary-preserving isometry' is a new mathematical operation on a finite region of a solid that transforms mathematically a given solid to a locally similar one. It is shown further that the existence of such a 'boundary-preserving isometry' in a given solid has infinitely many 'locally similar' solids as a consequence. Chemical implications, referring to the similarity of X-ray powder patterns and patent registration, are discussed as well. These theoretical concepts, which are first introduced in a schematic manner, are proved to exist in nature by the elucidation of the crystal structure of some diketopyrrolopyrrole (DPP) derivatives with surprisingly similar powder patterns. Although the available powder patterns were not indexable, the underlying crystals could be elucidated by using the new technique of ab initio prediction of possible polymorphs and a subsequent Rietveld refinement. Further ab initio packing calculations on other molecules reveal that 'local crystal similarity' is not restricted to DPP derivatives and should also be exhibited by other molecules such as quinacridones. The 'boundary-preserving isometry' is presented as a predictive tool for crystal engineering purposes and attempts to detect it in crystals of the Cambridge Structural Database (CSD) are reported.

The NMR-spectroscopic and X-ray crystal-structural characterization of two Cp*Ir halfsandwich complexes containing the 1,2-dicarba-closo-dodecaborane-1,2-diselenolato ligand

The reaction of [Cp*IrCl2](2) with dilithium 1,2-orthocarborane-1,2-diselenolate 3 leads to the green 16-electron diselenolene complex [Cp*Ir{Se2C2(B10H10)}] (4) which takes up two-electron ligands such as trimethylphosphane to give the 18-electron diselenolate derivative [Cp*Ir(PMe3)-{Se2C2(B10H10)}] (5). The molecular structures of 4 and 5 were determined by X-ray crystal structure analysis. The Se-77-nuclear shielding in 4 is lower by almost 500 ppm relative to that in 5.

X-Ray Photoelectron Spectroscopy Study of LaMn1-xFexO3 (x=0-1) Oxides

The redox potential, surface composition and oxygen species of a series of complex oxides LaMn1-xFexO3 (x=0-1) having perovskite structure (ABO(3)) have been investigated by means of XI'S. The variation of binding energies referring to Mn2p and Fe 2p under different treatment offerred an obvious evidence of redox between Mn and Fe, which could be expressed as Mn4+ + Fe(3-delta)+ Mn(4-delta)+ Fe3+ Feat Through computer fit three kinds of adsorbed oxygen species (O-I, O-II, O-III) have been evaluated based on the XPS spectra of O1s. From the variation of contents of different oxygen species, it could be concluded that. the redox occuring in the surface might be related with the adsorbed oxygen species O-I and O-II, furthermore the possibility of transfer of electron between adsorption site and oxygen was also discussed.

SMALL-ANGLE X-RAY-SCATTERING STUDY ON THE INTERFACE IN BLOCK-COPOLYMERS WITH FRACTAL PROPERTIES

The interface thickness in two triblock copolymers were determined using small-angle x-ray scattering in the context of the theory proposed by Ruland. The thickness was found to be nonexistent for the samples at three different temperatures. By viewing th

In situ high temperature X-ray diffraction studies of mixed ionic and electronic conducting perovskite-type membranes

Phase structure and stability of three typical mixed ionic and electronic conducting perovskite-type membranes, SrCo0.8Fe0.2O3-delta (SCF), Ba0.5Sr0.5Co0.8Fe0.2O3-delta (BSCF) and BaCo0.4Fe0.4Zr0.2O3-delta (BCFZ) were studied by in situ high temperature X-ray diffraction at temperatures from 303 to 1273 K and under different atmospheres (air, 2% O-2 in Ar and pure Ar) at 1173 K. By analyzing their lattice parameters the thermal expansion coefficients (TECs) of BSCF, SCF and BCZF are obtained to be 11.5 x 10(-6) K-1, 17.9 x 10(-6) K-1 and 10.3 x 10(-6) K-1, respectively. A relationship between phase stability and TEC was proposed: the higher is the TEC, the lower is the operation stability of the perovskite materials. (C) 2005 Elsevier B.V. All rights reserved.

Thermal mismatch stress in SiC whisker reinforced aluminium composite: new measurement method by X-ray diffraction

A new X-ray diffraction method for characterising thermal mismatch stress (TMS) in SiC_w–Al composite has been developed. The TMS and thermal mismatch strain (TMSN) in SiC whiskers are considered to be axis symmetrical, and can be calculated by measuring the lattice distortion of the whiskers. Not only the average TMS in whiskers and matrix can be obtained, but the TMS components along longitudinal and radial directions in the SiC whiskers can also be deduced. Experimental results indicate that the TMS in SiC whiskers is compressive, and tensile in the aluminium matrix. The TMS and TMSN components along the longitudinal direction in the SiC whiskers are greater than those along the radial direction for a SiC_w–Al composite quenched at 500°C.

X-Ray Observation on Flow and Failure of Saturated

介绍脉冲X光机和医用X光机的特性,应用这两种设备进行一系列饱和砂土的冲击加载实验。利用医用X光机拍摄到了饱和砂土在冲击载荷作用下产生的横断裂缝、纵向排水通道以及密实沉降的照片,得到了横断裂缝和纵向排水通道的出现规律,从而为研究饱和砂土冲击液化后结构破坏与密实沉降的机理提供了一种实验观测手段。