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Figure 2. Resistance measurement cell for membranes in a confined environment. The water flow goes through the channels on the bottom plate (shown in the left rear). The membrane sits between the two plates and absorbs water. The polycarbonate plates sit beneath the load washer. The membrane resistance (Rm) is determined across the stain- less steel electrode in the upper plate. The cell is compressed: a screw drive compresses a spring in the blue cylinder above the load washer (right). ent temperatures from 25 to 75 8C. The membranes weredriedinanovenat1308Cfor1handusedim- mediately. Dry samples were suspended on a Teflon thread from a bottom weighing balance. After the determination of the dry weight, the sample was positioned inside a three-necked flask half-filled with water. The flask temperature was controlled by a heating tape wrapped around the flask. A ther- mocouple was positioned in one neck of the flask to monitor the temperature. The temperature was con- stant to 61.5 8C over the course of the experiment. The mass increase was recorded as a function of time for $4000–5000 s. A combination temperature/ relative humidity (RH) sensor placed where the membrane samples normally hanged verified that the test conditions were 95–100% RH and the same temperature reported by the thermocouple. Membrane Proton Conductivity A polymer membrane in a fuel cell is in a con- strained environment under compression. To examine the effect of compression on the proton conductivity, the apparatus shown in Figure 2 was built. Polymer dog bones were placed in the com- pression cell shown in Figure 2(A). The bottom platehadtwo1mm1mm15mmchannels with water running through them. The top plate had two stainless steel cross bars machined flush with the polycarbonate, which ran perpendicularly to the water flow channel in the bottom plate. The central section of the dog bone was positioned Journal of Polymer Science: Part B: Polymer Physics DOI 10.1002/polb between the two flow channels. The flow channels were filled with water to maintain the water activ- ity in the membrane at unity (the membranes did not lose any water by evaporation during the com- pression measurements). Three types of measurements were performed: (1) the membrane resistance was measured as a function of the compressive stress on the mem- brane, (2) the membrane resistance was measured as a function of time at a constant stress, and (3) the membrane resistance was measured as the constrained membrane absorbed water. In the first experiment, the stress was increased from 0 to 7.25 MPa in incremental steps every minute, and then the pressure was reduced back to 0 in the reverse sequence. The entire cycle took 20 min. The second experiment consisted of permitting the membrane to equilibrate for $2 h at a fixed stress and then changing the stress and following the re- sistance as a function of time. For the third set of experiments, rectangular samples (5 cm 2.5 cm) were prepared with two 2.5 mm 20 mm slots cut out of the membrane in the area of the water flow channels. A load was imposed on the top plate [Fig. 2(B)]. The force of the load was measured via a load washer. A heavy-duty die spring kept the applied load fixed while allowing the membrane to expand or contract with the water uptake. The resistance of the membrane was measured by the application of an ac voltage across the membrane in series with a 1-kO resistor. The ac voltages across the TITANIA/NAFION COMPOSITE MEMBRANES 2331PDF Image | Properties of Nafion and Titania Nafion Composite Membranes
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