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An appropriate amount of the CNF suspension was added to the PDLLA suspension, stirred for 1 h, and immediately vacuum filtered using Millipore Durapore PVDF membrane filters with 90 mm in diameter and 0.65 ¦Ìm in pore size (Fisher Scientific, Pittsburgh, PA). The paste collected on the filter membrane was air-dried for 2−3 days. The dried sample cake was found to have a two-layered structure consisting of a self-standing PDLLA-filled CNF sheet on top of a loosely bonded layer of precipitated microparticles. The bottom layer of the microparticles would crumble into fine powder when pressed by hand and could be dissolved into ethyl acetate as a clear solution, showing no sign of CNF presence. The PDLLA-CNF sheets were removed from the cakes and were compression-molded using stainless-steel picture-frame molds (1.4 mm thick) on a Carver Laboratory Press (Carver Inc., Wabash, IN) at 105 ¡ãC and 90 psi (0.6 MPa). Three composites were prepared. Their actual weight contents were calculated to be 8, 15, and 32% by dividing the dry weight of the loaded CNF by the weight of the molded composites. The 8 and 15 wt % samples were prepared by molding six and five layers of sheets stacked together. Because a higher CNF content led to a higher amount of microparticles retained in the cellulose gel formed during the filtration and, in turn, a thicker PDLLA-CNF sheet obtained, the 32 wt % composite was molded from just one sheet. A control sample was made by filtering a PDLLA suspension and compression molding using the same procedure. |
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