Regenerated cellulose fibres, spun from a liquid crystalline precursor, were pyrolysed at temperatures in the range 400-2,500°C. Raman spectroscopy and X-ray diffraction showed that the degree of graphitisation of the fibre increased with increasing temperature. Electron microscopy, however, suggested that the fibres have a skin-core structure. This observation was confirmed by micro-Raman analysis, whereupon the ratio of the intensities of the D and G bands shows that the skin consists of a graphitised structure, whereas the core consists of significantly less graphitised material. The contributions of the graphitised skin and the inner core to the potential mechanical properties of the fibres were also assessed by following the position of the 2D Raman band during tensile deformation of the fibre. The Raman band shift rate against strain was used to evaluate the fibre modulus, which suggested a modulus of *140 GPa for the skin and 40 GPa for the core, respectively. If this incomplete graphitisation could be overcome, then there is potential to produce carbon fibres from these novel precursor materials.
The determination of the crystal orientation of regenerated cellulose fibers produced under different drawing regimes is presented. Orientation is determined by using wide-angle X-ray diffraction from a synchrotron source and by measuring the azimuthal width of equatorial reflections. The orientation parameter theta is then determined to compare fiber samples. By using a 500 nm beam size, clear differences between the crystal orientations of the skin and the core of the fibers are reported for a range of differently processed fibers for the first time. These results are shown to have implications for the mechanical properties of regenerated cellulose fibers. By applying tensile deformation to fiber bundles it is shown that the most misoriented samples undergo rapid decreases in the orientation parameter, which is an indication of crystal reorientation. However, the more highly oriented fibers undergo little reorientation. An average shear modulus for these fibers is determined by placing the data on a master curve and fitting with a model equation. By using another model for the fibers of low orientation and the shear modulus from the master curve analysis, it is shown that the deformation of less oriented fibers is dominated by shear between crystals, whereas the more oriented filaments are likely to undergo more significant chain deformation. By using a new model for fibers of low orientation, a parameter ksigma is introduced that gives the proportion of the fiber stress that is due to crystal shear. Systematic differences between this parameter for fibers of increasing initial orientation are reported. Moreover it is shown that the fibers of initially lower average orientation are governed by uniform strain, in agreement with the new model, whereas more highly oriented fibers deform under uniform stress. Furthermore, the model that we propose for misoriented domains and the use of a new factor dictating the proportion of shear stress may have general applications in materials engineering.
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