A pinhole small-angle x-ray scattering (SAXS) instrument was constructed at the SUNY X3A2 beamline, National Synchrotron Light Source, Brookhaven National Laboratory. The three pinholes were mounted in a thick-walled stainless steel pipe and prealigned by using a portable laser source and a charge-coupled device (CCD) area detector. After the prealignment, incorporation of the collimator to the synchrotron x-ray source required only maximization of the incident x-ray intensity passing through the pinholes, which could be done easily by using a scintillation counter after proper attenuation. The entire synchrotron SAXS instrument setup took only a few hours even without stepping motor control for the pinhole collimator unit. By combining this collimator with a CCD-based x-ray area detector which could be assembled by using commercially available components, the SAXS instrument showed good performance for structural scales up to an order of 100 nm. The CCD-based x-ray area detector used a computer- (or manually) controlled intensified unit with a variable gain setting in order to accommodate the changing x-ray flux and to protect the detector from over exposure, a necessary feature for operation of an area detector at a synchrotron light source.
Online studies of structure and morphology development during continuous drawing of a nylon 66 fiber at different temperatures were carried out using synchrotron wideangle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) techniques. From the two-dimensional (2D) WAXD measurement, unit-cell parameters were determined. The results confirm that the triclinic cell structure persists above the Brill transition temperature (about 443 K). With increasing temperature, the unit-cell dimension a (dominated by hydrogen bonding) remains almost unchanged, while b increases and c decreases (both show a step-change at 403 K, prior to the Brill transition). The constant value of a agrees with the argument that the hydrogen bonding is relatively immobile at high temperatures prior to melting. The step-changes in b and c suggest that a premelting process of small (or defective) crystals precedes the Brill transition. As a result, the anisotropic thermal expansion of the surviving larger crystals results in a step-change behavior. This hypothesis is consistent with the crystal density data as well as the morphology evaluation by SAXS. Several dimensions were extracted from the 2D SAXS data: lamellar crystal and amorphous thicknesses (along the fiber) determined by the correlation function method, and crystal fibril width (perpendicular to the fiber) determined by the Porod analysis. These results also indicate that drawing annihilates small crystals, but the strain effect is much less than the temperature effect.
A Bonse–Hart ultrasmall-angle x-ray scattering (USAXS) instrument has been designed, constructed, and tested employing a synchrotron x-ray source. The instrument permits experiments ranging from below 0 °C up to about 400 °C, as well as temperature scanning, jumping, quenching, and annealing experiments. The mechanical elements used Super Invar as the basic building material in order to minimize the thermal expansion effect. As the synchrotron beam after the beamline optics is already somewhat collimated and monochromatized, a very fine tuning of the first crystal was necessary. The high-temperature Bonse–Hart instrument increased the performance by a factor of about 10 when compared with our earlier room-temperature Bonse–Hart instrument using the same set of channel-cut germanium crystals. The instrument was tested by using a suspension of polystyrene latex spheres and by combining the USAXS measurement, for the first time, with measurements of the same latex suspension by means of laser light scattering.
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