Title: Micro-Waxs Study of Structural Heterogeneity in Single Pan-Precursor and Subsequent Carbon Fiber
Authors: C. Creighton, P. Lynch, S. Nunna, B. Fox, M. de Jong, and S. Mudie
Abstract: The crystallographic orientation distribution and micro-voids in polyacrylonitrile (PAN) based carbon fiber play a key role in controlling the fiber’s strength and modulus. The evolution of microstructure from polyacrylonitrile (PAN) precursor fibers throughout oxidation and subsequent carbon fiber, processed using a 100 ton carbon fiber pilot line (Carbon Nexus, Deakin University), was studied by synchrotron wide angle X-ray scattering (WAXS). A dedicated fiber testing capability has been developed on the X-ray Fluorescence Microscopy beamline at the Australian synchrotron facility, where spatially resolving measurements (Micro-WAXS patterns) were recorded as each single fiber was translated across the focused incident X-ray probe in 1 micron steps. Probing along the lateral fiber direction, (100) and (002) WAXS patterns for the PAN and subsequent carbon fibers respectively revealed a non-uniform distribution of crystallographic properties - quantified in terms of the lattice d-spacing, crystallite size and crystallographic orientation, indicating a skin-core-structure.
References:  Kobayashi, T., Sumiya, K., Fujii, Y., Fujie, M., Takahagi, T., Tashiro, K. “Stress-induced microstructural changes and crystallite modulus of carbon fiber as measured by X-ray scattering”, Carbon 50(3) (2012) 1163-1169. https://doi.org/10.1016/j.carbon.2011.10.029  F. Liu, F., Wang, H., Xue, L., Fan, L., Zhu, Z. “Effect of microstructure on the mechanical properties of PAN-based carbon fibers during high-temperature graphitization”, Journal of Materials Science 43(12) (2008) 4316-4322.  Liu, X., Zhu, C., Guo, J., Liu, Q., Dong, H., Gu,Y., Liu, R., Zhao, N., Zhang, Z., Xu, J. “Nanoscale dynamic mechanical imaging of the skin–core difference: From PAN precursors to carbon fibers”, Materials Letters 128(0) (2014) 417-420. https://doi.org/10.1016/j.matlet.2014.04.176  Yu, M.-J., Wang, C.-G., Bai, Y.-J., Wang, Y.-X., Zhu, B. “Evolution of tension during the thermal stabilization of polyacrylonitrile fibers under different parameters” Journal of Applied Polymer Science, 102 (2006), pp. 5500-5506. https://doi.org/10.1002/app.23960  Ko, T.H. “Influence of continuous stabilization on the physical properties and microstructure of PAN-based carbon fibers” Journal of Applied Polymer Science, 42 (1991), pp. 1949-1957. https://doi.org/10.1002/app.1991.070420719  Fu, Z., Gui, Y., Cao, C., Liu, B., Zhou, C., Zhang, H. “Structure evolution and mechanism of polyacrylonitrile and related copolymers during the stabilization”, Journal of Materials Science 49(7) (2014) 2864-2874.  Dalton, H., Heatley, F., Budd, P.M. “Thermal stabilization of polyacrylonitrile fibers”, Polymer 40(20) (1999) 5531-5543. https://doi.org/10.1016/S0032-3861(98)00778-2  Kobayashi, T., Sumiya, K., Fujii, Y., Fujie, M., Takahagi, T., Tashiro, K. “Stress concentration in carbon fiber revealed by the quantitative analysis of X-ray crystallite modulus and Raman peak shift evaluated for the variously-treated monofilaments under constant tensile forces”, Carbon 53(0) (2013) 29-37. https://doi.org/10.1016/j.carbon.2012.10.012  Kobayashi, T., Sumiya, Fukuba, Y., M. Fujie, M., Takahagi, T., Tashiro, K. “Structural heterogeneity and stress distribution in carbon fiber monofilament as revealed by synchrotron micro-beam X-ray scattering and micro-Raman spectral measurements”, Carbon 49(5) (2011) 1646-1652.  Loidl, D., Paris, O., Rennhofer, H., Müller, M., Peterlik, H. “Skin-core structure and bimodal Weibull distribution of the strength of carbon fibers”, Carbon 45(14) (2007) 2801-2805.  Liu, W.R. X. D. “X-ray studies on the structure of polyacrylonitrile fibers”, Macromolecules 26(12) (1993) 3030-3036. https://doi.org/10.1016/j.carbon.2007.09.011  Arbab, S., Mirbaha, H., Zeinolebadi, A., Nourpanah, P. “Indicators for evaluation of progress in thermal stabilization reactions of polyacrylonitrile fibers”, Journal of Applied Polymer Science 131(11) (2014) DOI: 10.1002/APP.40343. https://doi.org/10.1002/app.40343  Zhu, C. Liu, X., Mao, Y. Liu, R., Zhao, N., Zhang, X., Xu, J. 2D SAXS/WAXD analysis of PAN carbon fibre microstructure in organic/inorganic transformation”, Chinese Journal of Polymer Science (CJPS) 31(5) (2013) 823-832.  Yu, M.-J., Bai, Y.-J., Wang, C.-G., Xu, Y., Guo, P.-Z. “A new method for the evaluation of stabilization index of polyacrylonitrile fibers”, Materials Letters 61(11-12) (2007) 2292-2294. https://doi.org/10.1016/j.matlet.2006.08.071
Conference: SAMPE 2019 - Charlotte, NC
Publication Date: 2019/05/20
Price: FREEGet This Paper