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High performance carbon fibers from mesophases produced by supercritical fluid extraction

Posted on:1998-03-24Degree:Ph.DType:Dissertation
University:Clemson UniversityCandidate:Dauche, Franck MichelFull Text:PDF
GTID:1461390014477110Subject:Engineering
Abstract/Summary:
The purpose of this research is to investigate the potential of supercritical fluid extraction for the production of an improved precursor for the manufacture of high thermal conductivity carbon fibers. Mesophase pitch fractions were produced by the continuous fractionation of an isotropic petroleum-based pitch with supercritical toluene in a region of liquid-liquid equilibrium. A statistical experimental design was used to investigate a region of extraction operating conditions from which the fractions were expected to exhibit superior spinnability. Chemical and physical characterizations were performed on the fractions, and the results were used to explore the effect of the extraction conditions on the mesophase properties. DRIFT data were shown to be particularly useful for characterizing the chemical composition of the mesophase fractions produced, and GPC was successfully used to determine their molecular weight distribution.; Two thermodynamic models based on the SAFT equation together with (1) the concepts of continuous thermodynamics (2) molecular weight information on the oligomeric nature of the feed pitch were used to correlate the measured results. By using three adjustable parameters, solvent compositions and molecular weight distributions in each phase were calculated. Although the oligomeric model is able to qualitatively represent trends observed in the data, it cannot as yet be used to quantitatively predict phase compositions.; Based on the characterizations of the supercritically extracted mesophases produced, selected fractions were melt-spun into round- and ribbon-shaped fibers using a laboratory-scale melt-spinning apparatus. It was found that a relatively narrow window of mesophase properties and compositions allowed fiber making without off-gassing. For a given spinnable mesophase, wide angle X-ray diffraction was used on as-spun fibers produced over a wide range of spinning temperatures to evaluate their potential to yield, after proper heat treatment, carbon fibers exhibiting superior transport properties. True statistical differences in the as-spun orientation (Z value) of two fiber sets spun from the same mesophase yielded, upon identical heat treatment, true differences in tensile moduli, electrical resistivity, and crystallographic parameters.; Even though the heat treatment of the as-spun fibers was not optimized, final fibers with properties equal to those exhibited by Amoco's P-120 fibers were produced.
Keywords/Search Tags:Fibers, Produced, Mesophase, Supercritical, Extraction
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