Density estimations and comparisons of a fragmented single fiber using X-ray computed tomography.

A commercial X-ray computed tomography (CT) apparatus using a quasi-monochromatic beam was utilized for density estimations and comparisons of a fragmented single fiber. The validation of quasi-monochromaticity of the X-ray source was investigated by radiograph measurements. For the case of a transmittance higher than 50%, the contribution of Cu Kα characteristic X-rays was dominant. To realize a sufficient statistical quality, an attempt to increase the number of averaged voxels was demonstrated using the neighboring slices of the 3D-CT image. A minimum value of the coefficient of variation (CV) was achieved using multiple images rather than using a single image. The observed values of the inverse of the transmitted X-ray intensity (CT value) of the polymers showed a fairly good relationship with their density. An analytical curve derived from measurements of reference samples of known densities could provide the relative density of an unknown fragmented fiber down to the size of 30 µm in diameter and 35 µm in length. The CV of the estimated density was from 1.5 to 2%, which was estimated from the CV of CT values. Moreover, the correlation of CT values was improved with the linear absorption coefficient than the density. A better performance of discrimination of polymers including fibers might be realized with the difference of linear absorption coefficients for X-rays.

Non-destructive analysis of hollow-shaped single fibers using X-ray computed tomography.

A commercial high-resolution X-ray computed tomography (CT) was utilized for non-destructive analysis of single fibers. The micro-CT apparatus was employed because it is applicable to both colored and colorless fibers. A sample preparation using adhesive sheets was demonstrated, and the method is similar to typical tape-lift sample collection method in crime cases. Different cross-sectional shapes of nylon and polyester single fibers were non-destructively distinguished, and the method is applicable to all types of fibers. Cross-sectional areas, aperture ratios, and volumes of individual fibers were directly and automatically measured using the open-source software. The observed parameters were within a coefficient of variation of 3%. In addition, a mass of a single fragment of a fiber can be estimated when the local density is given.

In situ characterization of crystallization and melting of soft, thermoresponsive microgels by small-angle X-ray scattering.

Depending on the volume fraction and interparticle interactions, colloidal suspensions can form different phases, ranging from fluids, crystals, and glasses to gels. For soft microgels that are made from thermoresponsive polymers, the volume fraction can be tuned by temperature, making them excellent systems to experimentally study phase transitions in dense colloidal suspensions. However, investigations of phase transitions at high particle concentration and across the volume phase transition temperature in particular, are challenging due to the deformability and possibility for interpenetration between microgels. Here, we investigate the dense phases of composite core-shell microgels that have a small gold core and a thermoresponsive microgel shell. Employing Ultra Small-Angle X-ray Scattering, we make use of the strong scattering signal from the gold cores with respect to the almost negligible signal from the shells. By changing the temperature we study the freezing and melting transitions of the system in situ. Using Bragg peak analysis and the Williamson-Hall method, we characterize the phase transitions in detail. We show that the system crystallizes into an rhcp structure with different degrees of in-plane and out-of-plane stacking disorder that increase upon particle swelling. We further find that the melting process is distinctly different, where the system separates into two different crystal phases with different melting temperatures and interparticle interactions.

Feasibility Studies of X-Ray Computed Tomography for Forensic Examination of Single Fibers.

Non-destructive observations of cross-sectional shapes of acrylic single fibers using X-ray computed tomography (CT) were performed. A commercial X-ray CT apparatus (Rigaku nano3DX) was employed because of its micrometer-scale spatial resolution and remarkable image contrast for soft matter. We assessed two types of sample support, a paraffin strip and a nylon string, for single fiber samples in terms of easy handling and sample recovery. Fixed individual single fibers were loaded into a narrow polyimide tube in both cases, and the tube ensured that the sample remained in the field of view during the CT measurements. In both cases, the cross-sectional shapes of individual single fibers could be distinguished, with a circular shape for one sample and a triangular shape for the other. However, the support using a nylon string was found to be more suitable for further analysis. The cross-sectional profile of the obtained tomographic image showed a clear difference between polyimide and nylon. The intensity ratio or the image contrast corresponded to that of the local densities. It was also found that the effect of the artifact appeared at around the boundaries of the objects, but the local density could still be utilized for examining individual single fibers.

Local- and Intermediate-Range Structures on Ordinary and Exotic Phase-Change Materials by Anomalous X-ray Scattering.

Local- and intermediate-range atomic structures were investigated on amorphous phases of an ordinary phase-change material, Ge2Sb2Te5 (GST), and an exotic one, Cu2GeTe3 (CGT), by using anomalous X-ray scattering close to K absorption edges of each element to find a fast amorphous-crystalline phase-change mechanism. The obtained data were analyzed by using reverse Monte Carlo modeling to obtain partial structure factors, partial pair distribution functions, and three-dimensional atomic configurations. Ring statistics were carefully examined to clarify the similarity and difference compared with the corresponding crystal structures, and it was found that amorphous GST has a number of four-membered rings indicating fragments of crystal structure, and amorphous CGT has a remarkable number of three-membered rings showing a collapse of crystal structures composed of purely six-membered rings. A persistent homology analysis was carried out and long-range ring structures of the constituent elements were observed in the amorphous phase, which may originate from fragments of crystal structures with a long-range periodicity.