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2330 SATTERFIELD ET AL. Ziploc bag were clamped in the grips of the Ins- tron. The Ziploc bag was kept slack so it added a negligible contribution to the stress when each sample was strained. The membrane water con- tent during the test was determined by the weigh- ing of the sample before and after the test. The dry weight of the sample was determined after drying at 170 8C for 24 h. All tested samples contained Nafion EW 1100, so the water content per sulfonic acid residue (k) was calculated with eq 3: ðMTest MDryÞ 1 mole H2O 18:015 g H2O ð3Þ MDryð1Wt%TiO2Þ EWg Membrane=mol SO3 where MTest is the mass (g) of the sample during the test and MDry is the mass after drying at 1708Cfor24h. The Young’s modulus and plastic modulus were determined for each sample and plotted as a func- tion of the temperature and k value. (The plastic modulus, as we apply the term, refers to the change in the stress with strain beyond the yield point, which is a measure of the strain hardening of the material.) The tested membranes included extruded Nafion, Nafion recast with 0, 0.5, 1, 3, 6, or 20 wt % TiO2 and purchased from Degussa- Huls, Nafion recast with 3% TiO2 and purchased from Alfa-Aesar, Nafion recast with 3% rutile nee- dles, and Nafion recast with 3% Degussa-Huls TiO2 with the solvents IPA, DMSO, and EtOH. Although different solvents were tested, we saw no distinction between the membranes cast from these three solvents. Creep Testing The effect of a constant stress on the different membrane materials was evaluated by the mea- surement of their creep. The membranes were cut into ASTM standard dog-bone samples with a gauge length and width of 2.2 cm and 0.5 cm, respectively. Polymer dog bones of 115 membranes were cut and clamped in the apparatus shown in Figure 1. The entire apparatus was placed inside an acrylic box with beakers of saturated salt water baths to control the water activity, and the acrylic box was placed in an oven. A weight was hung from the bottom of the dog bone, and the polymer strain was recorded as a function of time. Dynamic Water Uptake and Conductivity Water sorption by Nafion and Nafion/titania com- posite membranes was measured at several differ- Journal of Polymer Science: Part B: Polymer Physics mol H O k 2 1⁄4 mol SO3 Apparatus for creep measurements of poly- mer membranes. The entire apparatus fit inside an acrylic box and was placed in an oven. changes in resistance, the membrane was made one leg of a voltage divider. A driving voltage of 100 Hz was applied across the membrane in series with a fixed 1-kO resistor. A pair of ac voltmeters measured the voltage drops across the membrane and the membrane in series with the fixed resistor. The dynamics of the change in the resistance of the membrane could be determined with a re- sponse time of $0.5 s. Mechanical Testing Tensile Tests The membranes were cut into ASTM standard dog-bone samples with a gauge length of 2.2 cm and a width of 0.5 cm. The samples were tested in an Instron with a constant strain rate of 5 cm/min. The testing chamber was heated to temperatures in the range of 20–120 8C. The water content was varied by the preconditioning of the samples in controlled-humidity environments (above satu- rated salt solutions). At room temperature, the water evaporation was sufficiently slow that the water content per sulfonic acid group did not change by more than 2 during the test. To test samples at higher temperatures without the loss of water, the dog bones were positioned inside a Ziploc polyethylene bag, and the samples and Figure 1. DOI 10.1002/polbPDF Image | Properties of Nafion and Titania Nafion Composite Membranes
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