Miscibility, crystallization κinetics and real-time small-Angle x-ray scattering investigation of the semicrystalline morphology in thermosetting polymer blends of epoxy resin and poly(ethylene oxide)

Thermosetting polymer blends of poly(ethylene oxide) (PEO) and bisphenol-A-type epoxy resin (ER) were prepared using 4,4′-methylenebis(3-chloro-2,6-diethylaniline) (MCDEA) as curing agent. The miscibility and crystallization behavior of MCDEA-cured ER/PEO blends were investigated by differential scanning calorimetry (DSC). The existence of a single composition-dependent glass transition temperature (Tg) indicates that PEO is completely miscible with MCDEA-cured ER in the melt and in the amorphous state over the entire composition range. Fourier-transform infrared (FTIR) investigations indicated hydrogen-bonding interaction between the hydroxyl groups of MCDEA-cured ER and the ether oxygens of PEO in the blends, which is an important driving force for the miscibility of the blends. The average strength of the hydrogen bond in the cured ER/PEO blends is higher than in the pure MCDEA-cured ER. Crystallization kinetics of PEO from the melt is strongly influenced by the blend composition and the crystallization temperature. At high conversion, the time dependence of the relative degree of crystallinity deviated from the Avrami equation. The addition of a non-crystallizable ER component into PEO causes a depression of both the overall crystallization rate and the melting temperature. The surface free energy of folding σe displays a minimum with variation of composition. The spherulitic morphology of PEO in the ER/PEO blends exhibits typical characteristics of miscible crystalline/amorphous blends, and the PEO spherulites in the blends are always completely volume-filling. Real-time small-angle X-ray scattering (SAXS) experiments reveal that the long period L increases drastically with increasing ER content at the same temperatures. The amorphous cured ER component segregates interlamellarly during the crystallization process of PEO because of the low chain mobility of the cured ER. A model describing the semicrystalline morphology of MCDEA-cured ER/PEO blends is proposed based on the SAXS results. The semicrystalline morphology is a stack of crystalline lamellae; the amorphous fraction of PEO, the branched ER chains and imperfect ER network are located between PEO lamellae.

Conjugated linoleic acid decreases fat accretion in pigs evaluation by dual-energy X-ray absorptiometry

Thirty female Large White × Landrace pigs (average weight 57·2 (SD 1·9) kg) were allocated to one of six dietary treatments containing 0, 1·25, 2·5, 5·0, 7·5 or 10·0 g 55 % conjugated linoleic acids (CLA) isomers (CLA-55)/kg diet and fed for 8 weeks. Each pig was scanned at 0, 28 and 56 d and again at post slaughter using dual-energy X-ray absorptiometry (DXA) to determine the temporal pattern of body composition responses. Values determined by DXA were adjusted using regression equations generated from validation experiments between chemically and DXA-predicted values. Overall, there was a significant linear reduction in fat content with the increasing levels of CLA in the diet (P=0·007, P=0·011, P=0·008 at week 4, week 8 and for the carcass, respectively). The greatest improvement was recorded at the early stages of CLA supplementation and for the highest dose of CLA (week 4, -19·2 % compared with week 8, -13·7 %). In the first 4 weeks of feeding CLA, pigs receiving 10 g CLA-55/kg diet deposited 93 g less fat/d than pigs fed basal diets (P=0·002) compared with only 6 g less fat than control animals in the final 4 weeks. Lean content and lean deposition rate were maximised at 5 and 2·5 g CLA-55/kg diet for the first 4 weeks (P=0·016) and the final 4 weeks of treatment (P=0·17), respectively. DXA estimates of bone mineral content and bone mineral density were not affected by CLA supplementation throughout the experiment. These data demonstrate that dietary CLA decreases body fat in a dose-dependent manner and that the response is greatest over the initial 4 weeks of treatment.

A uniaxial tensile stage with tracking capabilities for micro X-ray diffraction applications

First results are presented for a uniaxial tensile stage designed to operate on a scanning micro X-ray diffraction synchrotron beamline. The new tensile stage allows experiments at typical loading cycles used in standard engineering stress–strain tests. Several key features have been implemented to support in situ loading experiments at the intragranular length scale. The physical size and weight of the load cell were minimized to maintain the correct working distance for the X-ray focusing optics and to avoid overloading the high-resolution raster scan translation stages. A high-magnification optical microscope and image correlation code were implemented to enable automated online tracking capabilities during macroscopic elongation of the sample. Preliminary in situ tensile loading experiments conducted on beamline 12.3.2 at the Advanced Light Source using a polycrystalline commercial-purity Ti test piece showed that the elastic–plastic response of individual grains could be measured with submicrometre spatial resolution. The experiments highlight the unique instrumentation capabilities of the tensile stage for direct measurement of deviatoric strain and observation of dislocation patterning on an intragranular length scale as a function of applied load.

In-situ studies of X-ray diffraction line profiles from strained copper foils

The development of an in-situ tensometer is described along with preliminary results of x-ray line profiles from copper foils under tensile stress. The tensometer was designed and constructed on the high resolution diffraction instrument, Station 2.3 at the synchrotron radiation source (SRS) Daresbury Laboratory, and is capable of collecting data in either symmetric or asymmetric geometry including transmission and reflection modes. Experiments were carried out using 18 J..Lm thick copper foil up to strain levels of 5 % using both symmetric reflection and symmetric transmission diffraction. All profiles displayed diffraction broadening and asymmetry which increased with strain. In addition, the asymmetry observed in symmetric transmission was associated with extended tails on the low angle side of the profiles, but in symmetric reflection data the opposite asymmetry was observed. In the analysis, the measured profiles were fitted using the software TOPAS, a fundamental parameters approach to profile fitting. The instrumental profile function was characterised and modelled using annealed LaB6 powder. The diffraction broadening was then determined by refining the convolution of a Voigt function, an asymmetric exponential function and a fixed instrument function to reproduce the observed broadened profiles. The integral breadth and asymmetry results display a strong order dependence and increase almost linearly with strain. The results were interpreted by assuming crystallite size broadening in combination with dislocation broadening arising from fcc a/2( 110) {Ill } dislocations.