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.

Quantitative assessment of through-thickness crack size based on Lamb wave scattering in aluminium plates

The interaction of Lamb wave modes at varying frequencies with a through-thickness crack of different lengths in aluminium plates was analysed in terms of finite element method and experimental study. For oblique-wave incidence, both numerical and experimental results showed that the wave scattering from a crack leads to complicated transmission, reflection and diffraction accompanied by possible wave-mode conversion. A dual-PZT actuation scheme was therefore applied to generate the fundamental symmetrical mode (S0) with enhanced energy to facilitate the identification of crack-scattered wave components. The relationship between crack length and the reflection/transmission coefficient obtained with the aid of the Hilbert transform was established, through which the crack length was quantitatively evaluated. The effects of wavelength of Lamb waves and wave diffraction on the properties of the reflection and transmission coefficients were analysed.

Technique for improving the reception of scattering signal behind an obstacle

This thesis presents a solution to the problem of receiving a signal in the shadow and fringe areas. Theoretical and experimental investigation of the field behind an obstacle in a line of sight transmission path for UHF / microwave signals has resulted in a new approach to the analysis of electromagnetic fields in the shadow of an obstacle. Analysis using this approach showed the field to consist of varying amplitude and phase distribution. Additional analysis predicted an increase in received signal could be achieved if correlation between the field and antenna structure could be obtained. This was accomplished with a new antenna design. The thesis presents experimental and photographic evidence to support the theory. A novel technique involving the matching of the antenna structure to the field distribution, resulted in an increase of received signal in the diffracted field of up to 4 dB.

Qualitative and quantitative analysis of lipid classes in fish oils by thin-layer chromatography with an Iatroscan flame Ionization detector (TLC-FID) and liquid chromatography with an evaporative light scattering detector (LC-ELSD)

Combined effects of hydrogen and air flow rates on the peak response of selected neutral lipid classes (triacylglycerol, diacylglycerol, monoacylglycerol, free fatty acids, and ethyl esters) were studied to optimize and calibrate the Iatroscan Mk-6s Chromarod system for the qualitative and quantitative analysis of lipid classes by thin-layer chromatography (TLC) with flame ionization detection in fish oil during the transesterification process. Air flow rate of 2 L/min, hydrogen flow rate of 150-160 mL/min, and scan rate of 30 s/rod were found to be the optimum conditions. All samples were also analyzed by high performance liquid chromatography (HPLC) with evaporative light scattering detection. Quantitative results obtained by TLC with the flame ionization detection method were comparable to those obtained from HPLC with evaporative light scattering detection.

Surface-enhanced raman scattering spectroscopy of resveratrol

We report here, for the first time, the surface-enhanced Raman scattering (SERS) spectra of resveratrol using KNO₃-aggregated citrate-reduced silver (Ag) colloids. The technique provided a substantial spectral enhancement and therefore good quality spectra of resveratrol at parts per million (ppm) concentrations. The detection limit was found to be <1 μM, equivalent to <0.2 ppm. The SERS profile additionally closely resembled its normal solid-state Raman spectrum with some changes in relative intensity. These intensity changes, together with a precise band assignment aided by density functional theory calculations at the B3LYP/6–31G(d) level, allowed the determination of the structural orientation of the adsorbed resveratrol on the surface of the metal nanoparticles. In particular, the SERS spectra obtained at different resveratrol concentrations exhibited concentration-dependent features, suggesting an influence of surface coverage on the orientation of the adsorbed molecules. At a high concentration, an adoption of close-to-upright orientation of resveratrol adsorbed on the metal surface through the p-OH phenyl ring is favoured. The binding structure is, however, altered at lower surface coverage when the concentration decreases to a tilted orientation with the trans-olefin C=C bond aligning closer to parallel to the surface of the Ag nanoparticles.

Modelling of fibre-diameter-dependent light scattering to determine diameter corrections for colour measurement of wool

In this paper, fibre-diameter-dependent light scattering during measurement of wool colour was quantified using the extended multiplicative signal correction technique. Furthermore, a simple-to-apply model has been developed to correct each of the CIE (International Commission on Illumination) X, Y and Z values obtained from colour measurement of fibrous masses. The model was successfully applied to both polypropylene (PP) and wool fibres, though different parameter values were used in each case, indicating different patterns of internal light scattering between PP and wool fibres. After the model corrections, the diameter dependence of measured wool yellowness (Y - Z) was either eliminated or significantly reduced for each of seven sheep flocks distributed widely over the wool-growing regions of Australia.

Plane wave scattering by a spherical di-electric particle in motion : a relativistic extension of the Mie theory

Light scattering from small spherical particles has applications in a vast number of disciplines including astrophysics, meteorology optics and particle sizing. Mie theory provides an exact analytical characterization of plane wave scattering from spherical dielectric objects. There exist many variants of the Mie theory where fundamental assumptions of the theory has been relaxed to make generalizations. Notable such extensions are generalized Mie theory where plane waves are replaced by optical beams, scattering from lossy particles, scattering from layered particles or shells and scattering of partially coherent (non-classical) light. However, no work has yet been reported in the literature on modifications required to account for scattering when the particle or the source is in motion relative to each other. This is an important problem where many applications can be found in disciplines involving moving particle size characterization. In this paper we propose a novel approach, using special relativity, to address this problem by extending the standard Mie theory for scattering by a particle in motion with a constant speed, which may be very low, moderate or comparable to the speed of light. The proposed technique involves transforming the scattering problem to a reference frame co-moving with the particle, then applying the Mie theory in that frame and transforming the scattered field back to the reference frame of the observer.

Analysing ordered nanostructures in epoxy thermosets using small angle X-ray scattering techniques

Small angle X-ray scattering (SAXS) is essential for the morphological investigation of nanostructured systems as it is a bulk sampling technique and provides information about the overall distribution of the components in the system. In our study we have used SAXS to identify various ordered and disordered morphologies in block copolymer modified epoxy thermosets. We have used a reactive block copolymer and hydrogen bonding block copolymer to modify epoxy resin (ER) to see the effect of various blocks on the morphological changes.

Compression and probing C−H···I hydrogen bonds of iodoform under high pressure by x-ray diffraction and raman scattering

High-pressure methods were applied to investigate the structural stability and hydrogen bonding of polar molecules of iodoform by synchrotron radiation X-ray diffraction and Raman spectra measurements, respectively. Up to a pressure of 40 GPa, no phase transitions were observed. The discontinuous frequency shift of the C−H stretching band is believed to be related to the enhancement of the C−H···I weak hydrogen bonds under high pressures. Ab initio calculations were performed, and the results predict the frequency shift of the C−H stretching vibration as C−H···I interacts via hydrogen bonding. The bulk modulus is 17.3 ± 0.8 GPa, with a pressure derivative of 5.2.