Probing structural changes of spin-coated polystyrene film after swelling and precipitation by synchrotron GIUSAXS and AFM

Polystyrenc film of about 50 nm in thickness on silicon wafer was obtained by spin-coating in tetrahydrofuran solution.The film exhibits a rough surface as shown by atomic force microscopy images and ellipsometry data.

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.

Synchrotron-laser interactions in hexagonal boron nitride: an examination of charge trapping dynamics at the boron K-edge

Poolton, Nigel; Towlson, B.M.; Hamilton, B.; Evans, D.A., (2006) 'Synchrotron-laser interactions in hexagonal boron nitride: an examination of charge trapping dynamics at the boron K-edge', New Journal of Physics 8 pp.76 RAE2008

Synchrotron-laser pump-probe luminescence spectroscopy: Correlation of electronic defect states with x-ray absorption in wide-gap solids

Poolton, Nigel; Hamilton, B.; Evans, D.A., (2005) 'Synchrotron-laser pump-probe luminescence spectroscopy: Correlation of electronic defect states with x-ray absorption in wide-gap solids', Journal of Physics D: Applied Physics 38 pp.1478-1484 RAE2008

Evidence of various mechanisms of Cd sequestration in the hyperaccumulator Arabidopsis halleri, the non accumulator Arabidopsis lyrata and their progenies by combined synchrotron-based techniques

Arabidopsis halleri is a model plant for Zn and Cd hyperaccumulation. The objective of this study was to determine the relationship between the chemical forms of Cd, its distribution in leaves, and Cd accumulation and tolerance. An interspecific cross was carried out between A. halleri and the non-tolerant and non-hyperaccumulating relative A. lyrata providing progenies segregating for Cd tolerance and accumulation. Cd speciation and distribution were investigated using X-ray absorption spectroscopy and microfocused X-ray fluorescence. In A. lyrata and non-tolerant progenies, Cd was coordinated by S atoms only or with a small contribution of O groups. Interestingly, the proportion of O ligands increased in A. halleri and tolerant progenies, and they were predominant in most of them, while S ligands were still present. Therefore, the binding of Cd with O ligands was associated with Cd tolerance. In A. halleri, Cd was mainly located in the xylem, phloem, and mesophyll tissue, suggesting a reallocation process for Cd within the plant. The distribution of the metal at the cell level was further discussed. In A. lyrata, the vascular bundles were also Cd enriched, but the epidermis was richer in Cd as compared with the mesophyll. Cd was identified in trichomes of both species. This work demonstrated that both Cd speciation and localization were related to the tolerance character of the plant.

Intermetallic phase detection in lead-free solders using synchrotron X-ray diffraction

The high-intensity, high-resolution x-ray source at the European Synchrotron Radiation Facility (ESRF) has been used in x-ray diffraction (XRD) experiments to detect intermetallic compounds (IMCs) in lead-free solder bumps. The IMCs found in 95.5Sn3.8Ag0.7Cu solder bumps on Cu pads with electroplated-nickel immersion-gold (ENIG) surface finish are consistent with results based on traditional destructive methods. Moreover, after positive identification of the IMCs from the diffraction data, spatial distribution plots over the entire bump were obtained. These spatial distributions for selected intermetallic phases display the layer thickness and confirm the locations of the IMCs. For isothermally aged solder samples, results have shown that much thicker layers of IMCs have grown from the pad interface into the bulk of the solder. Additionally, the XRD technique has also been used in a temperature-resolved mode to observe the formation of IMCs, in situ, during the solidification of the solder joint. The results demonstrate that the XRD technique is very attractive as it allows for nondestructive investigations to be performed on expensive state-of-the-art electronic components, thereby allowing new, lead-free materials to be fully characterized.

Synchrotron X-ray diffraction study of the phase transformations in titanium alloys

High-resolution synchrotron X-ray diffraction was used to study the phase transformations in titanium alloys. Three titanium alloys were investigated: Ti-6Al-4V, Ti-6Al-2Sn-4Zr-2Mo-0.08Si and beta21s. Both room and high temperature measurements were performed. The room temperature experiments were performed to study the structure of the alloys after different heat treatments, namely as received (AR), furnace cooling (FC), water quenching (WQ) and water quenching followed by ageing. The alpha, alpha', alpha'' and beta phases were observed in different combinations depending on the heat treatment conditions and the alloy studied. A multicomponent hexagonal close packed (hcp) alpha phase, with different c and the same a lattice parameters, was detected in Ti-6Al-4V after FC. High temperature synchrotron X-ray diffraction was used for 'in situ' study of the transformations on the sample surface at elevated temperatures. The results were used to trace the kinetics of surface oxidation and the concurrent phase transformations taking place under different conditions. The influence of the temperature and oxygen content on the lattice parameters of the alpha phase was derived and new data obtained on the coefficients of thermal expansion in the different directions of the hcp alpha phase, for Ti-6Al-4V and Ti-6Al-2Sn-4Zr-2Mo-0.08Si.

Polarisation analysis of VUV synchrotron radiation emitted from a bending magnet source in the energy range 20-50 eV: A comparison between measurements and theoretical predictions

The results of a study to characterise the polarisation properties of the photon beam emerging from beamline 5D, mounted on a bending magnet source at the Synchrotron Radiation Source, Daresbury Laboratory, are presented. The expectation values for the Stokes parameters corresponding to the light transmitted by the beamline have been calculated by combining ray-tracing and optical methods. The polarisation of the light at the source is modified both by the beamline geometry and by the reflections at the optical components. Although it is often assumed that the polarising properties of grazing incidence optics are negligible, this assumption leads to rather inaccurate results in the VUV region. A study of the reflectivity shows that even at incidence angles (theta(i) = 80-85degrees) which are far from the Brewster angle (theta(B) similar to 45degrees for VUV and soft X-ray radiation) the residual changes in the amplitudes of the reflected light can result in non-negligible polarisation effects. Furthermore, reflection at grazing incidence gives rise to a substantial change in the phase, and this has the effect of rotating the elliptically polarised state. Theoretical Stokes parameters have been compared with full polarisation measurements obtained using a reflection polarimeter in the energy range 20-40 eV. (C) 2003 Elsevier B.V. All rights reserved.

Multiaxial Deformation of Polyethylene and Polyethylene/Clay Nanocomposites: In Situ Synchrotron Small Angle and Wide Angle X-Ray Scattering Study

A unique in situ multiaxial deformation device has been designed and built specifically for simultaneous synchrotron small angle X-ray scattering (SAXS) and wide angle X-ray scattering (WAXS) measurements. SAXS and WAXS patterns of high-density polyethylene (HDPE) and HDPE/clay nanocomposites were measured in real time during in situ multiaxial deformation at room temperature and at 55 degrees C. It was observed that the morphological evolution of polyethylene is affected by the existence of clay platelets as well as the deformation temperature and strain rate. Martensitic transformation of orthorhombic into monoclinic crystal phases was observed under strain in HDPE, which is delayed and hindered in the presence of clay nanoplatelets. From the SAXS measurements, it was observed that the thickness of the interlamellar amorphous region increased with increasing strain, which is due to elongation of the amorphous chains. The increase in amorphous layer thickness is slightly higher for the nanocomposites compared to the neat polymer. (C) 2011 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 49: 669-677, 2011