Characterization of supported cylinder-planar germanium waveguide sensors with synchrotron Infrared radiation

Cylinder-planar Ge waveguides are being developed as evanescent-wave sensors for chemical microanalysis. The only non-planar surface is a cylinder section having a 300-mm radius of curvature. This confers a symmetric taper, allowing for direct coupling into and out of the waveguide's 1-mm² end faces while obtaining multiple reflections at the central <30-μm-thick sensing region. Ray-optic calculations indicate that the propagation angle at the central minimum has a strong nonlinear dependence on both angle and vertical position of the input ray. This results in rather inefficient coupling of input light into the off-axis modes that are most useful for evanescent-wave absorption spectroscopy. Mode-specific performance of the cylinder-planar waveguides has also been investigated experimentally. As compared to a blackbody source, the much greater brightness of synchrotron-generated infrared (IR) radiation allows a similar total energy throughput, but restricted to a smaller fraction of the allowed waveguide modes. However, such angle-selective excitation results in a strong oscillatory interference pattern in the transmission spectra. These spectral oscillations are the principal technical limitation on using synchrotron radiation to measure evanescent-wave absorption spectra with the thin waveguides.

Dispersion of boron nitride nanotubes in aqueous solution with the help of ionic surfactants

We report that ammonium oleate surfactants can help the dispersion of multiwalled boron nitride nanotubes (BNNTs) in water to form a BNNT solution stable for several months, which was due to the non-covalent functionalization of nanotube surfaces. Fourier Transform Infrared Spectroscopy (FTIR) and Photoluminescence (PL) analysis with synchrotron radiation source revealed that this BNNT aqueous solution preserves the intrinsic optical properties of BNNTs. © 2009 Elsevier Ltd. All rights reserved.

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.

Direct observation of the intergallery expansion of polystyrene–montmorillonite nanocomposites

The intergallery expansion development of a series of differently modified montmorillonite polystyrene nanocomposites was directly observed with time-resolved in situ small-angle X-ray scattering (SAXS) using synchrotron radiation. The results indicated that the interlayer expansion varied depending on the clay modification and the chemical compatibility of the clay modifiers with the styrene monomer. The influence of the differently modified clays on the free radical polymerization was also investigated, particularly the effect on the conversion of styrene and molecular weight evolution of the polymer. On the basis of the kinetic study of the polymerization of styrene in the presence of varied modified clay particles, the intergallery expansion mechanism was postulated and discussed for different composite morphologies. Such studies provide an important guideline for the design of clay modifiers and development of clay–polymer nanocomposites.

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.

Comparative studies of structural transition between AlN nanocrystals and nanowires

The structural transition of AIN nanocrystals and nanowires were investigated simultaneously under pressures up to 37.2 GPa by in situ angle dispersive high-pressure x-ray diffraction using synchrotron radiation source and a single diamond anvil cell. The size of hexagonal AIN nanocrystals and the diameter of nanowires are 45 nm on average. A pressure-induced wurtzite to rocksalt phase transition starts at 21.5 GPa and completes at 27.8 GPa for the nanocrystals and nanowires, respectively. The high-pressure behaviors of AlN nanocrystals the same as the AIN nanowires might arise from the similar size and diameter in nanocrystals and nanowires. Hexagonal AIN nanocrystals (45 nm) display an apparent volumetric contraction as compared to the AlN nanocrystals (10 nm) which might induce the difference of transition pressure.

In situ synchrotron SAXS study of polymerizable microemulsions

We present for the first time a real-time small-angle X-ray scattering (SAXS) study of the structural transition of fluid microemulsion to solid polymerized material in a silicone polymerizable microemulsion system. A reactive methacrylate-terminated siloxane macromonomer (MTSM, Mn ∼ 1000 g/mol) was synthesized and used for microemulsion formulations comprising MTSM (oil phase), water, and a mixture of nonionic surfactant (Teric G9A8) with isopropanol. In situ synchrotron SAXS was used to investigate time-dependent nanostructure evolution during the polymerization reaction, which was directly initiated by X-ray radiation. The SAXS data were analyzed using both the Teubner-Strey model and the core-shell model. The results obtained by the Teubner-Strey model showed that the domain size (d) decreased while the correlation length (ξ) increased upon polymerization. The analysis in terms of the core-shell model displayed that adding water to the precursor microemulsion caused the water droplets to start swelling, which resulted in the discontinuity of water in oil microemulsion. There exhibited large differences in morphologies of polymerized materials from the microemulsion formulations with different water and surfactant contents. The core and shell sizes of water droplets decreased during the course of polymerization when there was 15 wt % or more water in the microemulsion formulation; the polymerized material thus exhibited increasingly discrete granular morphology. When there was 10 wt % or less water content in the precursor microemulsion, the rearrangement of water domains could be minimized during the course of polymerization and transparent polymerized material was obtained.