Defense Date


Document Type


Degree Name

Master of Science


Chemical Engineering

First Advisor

Dr. Mark A. McHugh


This research project investigates a new technique to efficiently mix crystalline solid additives with polymers by gentle ball milling with steel balls in the presence of carbon dioxide (C02) at 17 to 30°C and 1300 to 2500 psig. As the ball milling system is agitated, the steel balls transfer mechanical energy to the fluoropolymer and additive thereby converting them to powders. C02 is added into the chamber to expand the polymer and make it amenable to impregnation by the additive. At the end of the mixing process, a free flowing powder is produced consisting of the additive coated with fluoropolymer. The additives were extracted from the powders and intrinsic viscosity measurements were done on the remnant fluoropolymer. Viscosity studies showed that the virgin and post-ball milled fluoropolymers had similar intrinsic viscosities, hence similar molecular weights within experimental error limits. This implies that most of the polymer chains were simply disentangled during the mixing process and not broken. Differential Scanning Calorimetry (DSC) and Thermal Gravimetric Analysis (TGA) were done on the virgin polymer, the additives and the fabricated powders to determine the loading levels and to ascertain if there were any changes to the physical properties of the polymer. Scanning electron micrographs showed that some of the powder particles had additive particles stuck on the surface, but when these additives were washed off the surface of the powders with a suitable solvent that did not dissolve the polymer, DSC analysis showed the presence of additive incorporated into the polymer matrix.


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Date of Submission

June 2008