Carbon fibers stabilization process

The carbon fiber production process involves a series of steps including spinning of the precursor fiber, stabilization, carbonization, and post-carbonization treatments that include sizing and surface treatments. The specifics of these steps vary greatly, depending on the precursor material and the desired properties of the carbon fiber. Figure 4 shows a schematic of the carbon fiber production process. 

More than 95% of current carbon fiber production for advanced composite appHcations is based on the thermal conversion of polyacrylonitrile (PAN) or pitch precursors to carbon or graphite fibers. Generally, the conversion of PAN or pitch precursor to carbon fiber involves similar process steps fiber formation, ie, spinning, stabilization to thermoset the fiber, carbonization—graphitization, surface treatment, and sizing. Schematic process flow diagrams are shown in Eigure 4. However, specific process details differ. 

Fibers produced from pitch precursors can be manufactured by heat treating isotropic pitch at 400 to 450°C in an inert environment to transform it into a hquid crystalline state. The pitch is then spun into fibers and allowed to thermoset at 300°C for short periods of time. The fibers are subsequendy carbonized and graphitized at temperatures similar to those used in the manufacture of PAN-based fibers. The isotropic pitch precursor has not proved attractive to industry. However, a process based on anisotropic mesophase pitch (30), in which commercial pitch is spun and polymerized to form the mesophase, which is then melt spun, stabilized in air at about 300°C, carbonized at 1300°C, and graphitized at 3000°C, produces ultrahigh modulus (UHM) carbon fibers. In this process tension is not requited in the stabilization and graphitization stages. 

The as-spun acrylic fibers must be thermally stabilized in order to preserve the molecular structure generated as the fibers are drawn. This is typically performed in air at temperatures between 200 and 400°C [8]. Control of the heating rate is essential, since the stabilization reactions are highly exothermic. Therefore, the time required to adequately stabilize PAN fibers can be several hours, but will depend on the size of the fibers, as well as on the composition of the oxidizing atmosphere. Their are numerous reactions that occur during this stabilization process, including oxidation, nitrile cyclization, and saturated carbon bond dehydration [7]. A summary of several fimctional groups which appear in stabilized PAN fiber can be seen in Fig. 3. 

One typical example of carbon/carbon composite plates is that made by Oak Ridge National Laboratory (ORNL) in the United States [12]. The composite preform was fabricafed by a slurry-molding process from fhe mixed slurry befween short carbon fibers (graphite fibers were also added in some sample plates) and fhe phenolic resin. The mass rafio between fiber reinforcement and phenolic matrix is 4 3. The phenolic matrix improves the mechanical properties and dimensional stability of the plate. A subsequent vacuum molding process was utilized to fabricate composite plates and fluid fields with relatively high resolution (Figure 5.3, [11]). 

Poly[2,2 -(m-phenylene-5,5 -benzimidazole)] (PBI) is a very high glass transition temperature (Tg 430°C), commercially available material. It possesses excellent mechanical properties, but is difficult to process into large parts and has high moisture regain and poor thermo-oxidative stability at temperatures above approximately 260 °C. Polyimides, especially the thermoplastic polyimides, offer attractive thermo-oxidative stability and processibility, but often lack the thermal and mechanical characteristics necessary to perform in applications such as the matrix for high use-temperature (over 300 °C) structural composites (for example, carbon fiber reinforced) for aerospace use. The attempt to mitigate... 

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