MODIFICATION OF POLYACRYLONITRILE (PAN)CARBON FIBER PRECURSOR VIA POST-SPINNING PLASTICIZATION AND STRETCHING IN DIMETHYL FORMAMIDE (DMF)

This study investigates the possibility of using a post-spinning plasticization and stretching process to eliminate suspected property-limiting factors in polyacrylonitrile-based carbon fibers. This process was performed with the intention of removing surface defects (to improve tensile strength), attenuating fiber diameter (to promote more uniform heat treatment), and reducing molecular dipole interactions (to facilitate further molecular orientation). Among the various organic and inorganic solutions tested, treatment using aqueous dimethyl formamide (DMF) offered far and away the best properties and was therefore selected for further testing. Tested individually (as single filaments), fibers exposed to 80% DMF for 10 s gave the highest precursor values of elastic modulus (9.07 GPa) and tensile strength (675 MPa). While fibers treated in 80% DMF gave a 73% improvement in elastic modulus and a 53% improvement in tensile strength over as-received PAN, limitations in sample preparation and carbonization necessitated a reduction in DMF concentration (to 30%) to allow extraction of individual carbon fibers for tensile testing. Despite this compromise, results for fibers carbonized at 1000°C ultimately showed a 32% improvement in carbon fiber elastic modulus and a 14% improvement in carbon fiber tensile strength over regularly prepared carbon fibers. These results show that, to a certain extent, improvements in PAN precursor properties can translate to corresponding improvements in subsequently produced carbon fibers. Additional characterization using wide angle X-ray scattering (WAXS) and scanning electron microscopy (SEM) suggests that these improvements are due in part to improved lateral order as well as the successful elimination of surface defects and prevention of skin-core formation.

[1]  R. Mathur,et al.  IR studies of PAN fibres thermally stabilized at elevated temperatures , 1994 .

[2]  Robert A. Meyers,et al.  Encyclopedia of physical science and technology , 1987 .

[3]  A. Abhiraman,et al.  Exploratory experiments in the conversion of plasticized melt spun PAN-based precursors to carbon fibers , 1988 .

[4]  M. Balasubramanian,et al.  Conversion of acrylonitrile-based precursors to carbon fibres , 1987 .

[5]  R. Mathur,et al.  Bimodification of polyacrylonitrile (PAN) fibers , 1993 .

[6]  W. Watt Carbon work at the royal aircraft establishment , 1972 .

[7]  A. Abhiraman,et al.  Conversion of acrylonitrile-based precursor fibres to carbon fibres , 1987 .

[8]  R. Mathur,et al.  Post spinning modification of PAN fibres — a review , 1997 .

[9]  R. Mathur,et al.  Modification of PAN precursor—Its influence on the reaction kinetics , 1988 .

[10]  J. Liu,et al.  Continuous carbonization of polyacrylonitrile-based oxidized fibers : aspects on mechanical properties and morphological structure , 1994 .

[11]  D. J. Johnson Structure-property relationships in carbon fibres , 1987 .

[12]  Erich Fitzer,et al.  The influence of oxygen on the chemical reactions during stabilization of pan as carbon fiber precursor , 1975 .

[13]  Tse-Hao Ko,et al.  Characterization of PAN precursor modified with potassium permanganate , 1988 .

[14]  R. Mathur,et al.  Advances in the development of high-performance carbon fibres from pan precursor , 1994 .

[15]  B. F. Jones,et al.  The effect of fibre diameter on the mechanical properties of graphite fibres manufactured from polyacrylonitrile and rayon , 1971 .

[16]  M. Dresselhaus,et al.  Graphite fibers and filaments , 1988 .

[17]  P. Wang,et al.  Physical modification of polyacrylonitrile precursor fiber: Its effect on mechanical properties , 1994 .

[18]  R. Mathur,et al.  Characteristics of KMnO4-modified PAN fibres : its influence on the resulting carbon fibres' properties , 1994 .

[19]  Tse-Hao Ko,et al.  Preparation of graphite fibres from a modified PAN precursor , 1992 .

[20]  S. Damodaran,et al.  Chemical and Physical Aspects of the Formation of Carbon Fibres from PAN-based Precursors , 1990 .

[21]  D. Uhlmann,et al.  Oxidative stabilization of acrylic fibres , 1979 .

[22]  S. Mukhopadhyay,et al.  Structure-Property Relationships of PAN Precursor Fibers During Thermo-oxidative Stabilization , 1995 .

[23]  E. Fitzer Pan-based carbon fibers—present state and trend of the technology from the viewpoint of possibilities and limits to influence and to control the fiber properties by the process parameters , 1989 .

[24]  Ko Tse-Hao,et al.  The effect of stabilization on the properties of PAN-based carbon films , 1993 .

[25]  Tse-Hao Ko,et al.  Influence of continuous stabilization on the physical properties and microstructure of PAN‐based carbon fibers , 1991 .

[26]  J. Bailey,et al.  Oxidation of Acrylic Fibres for Carbon Fibre Formation , 1973, Nature.

[27]  T. L. Dhami,et al.  Modification of polyacrylonitrile fibres to make them suitable for conversion into high performance carbon fibres , 1985 .

[28]  S. Peters Handbook of Composites , 1998 .

[29]  A. Abhiraman,et al.  Oxidative stabilization of oriented acrylic fibres—morphological rearrangements , 1983 .