Wet spinning of polyacrylonitrile‐based polymers is a common technique to manufacture carbon fiber precursors. Understanding the role of stretch profile on structural evolution will support efforts to reduce cost and improve process robustness. Fiber stretch generally occurs in three sequential stages: jet stretch, wet stretch (first draw), and hot draw (second draw). In this study, total fiber stretch was kept constant, but distributed differently across the stretch stages yielding three different fiber variants. Samples were collected and analyzed after each stretch stage in order to correlate process parameters to structural information. For all variants, orientation of the ordered phase increases gradually for each stage of stretch while activation energy for the structural relaxation decreases. Alternatively, crystallite size increases substantially during hot draw, which is shown to have the most pronounced effect on cyclization behavior. Given the process conditions, the variant with the lowest jet stretch and highest hot draw demonstrates the highest tenacity and modulus along with the greatest orientation, crystallite size, and highest peak exotherm temperature.
Carbon fiber precursor materials, such as polyacrylonitrile, pitch, and cellulose/rayon, require thermal stabilization to maintain structural integrity during conversion into carbon fiber. Thermal stabilization mitigates undesirable decomposition and liquification of the fibers during the carbonization process. Generally, the thermal stabilization of mesophase pitch consists of the attachment of oxygen‐containing functional groups onto the polymeric structure. In this study, the oxidation of mesophase pitch precursor fibers at various weight percentage increases (1, 3.5, 5, 7.5 wt%) and temperatures (260, 280, 290 °C) using in situ differential scanning calorimetry and thermogravimetric analysis is investigated. The results are analyzed to determine the effect of temperature and weight percentage increase on the stabilization process of the fibers, and the fibers are subsequently carbonized and tested for tensile mechanical performance. The findings provide insight into the relationship between stabilization conditions, fiber microstructure, and mechanical properties of the resulting carbon fibers.
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