Cryo-SEM of hydrated high temperature proton exchange membranes
- ORNL
Alternative energy technologies, such as high temperature fuel cells and hydrogen pumps, rely on proton exchange membranes (PEM). A chemically and thermally stable PEM with rapid proton transport is sol-gel phosphoric acid (PA)-doped polybenzimidazole (PBI) membranes. It is believed that the key to the high ionic conductivity of PA-doped PBI membranes is related to the gel morphology. However, the gel structure and general morphology of this PA-doped PBI membrane has not been widely investigated. In an effort to understand the gel morphology, two SEM sample preparation methodologies have been developed for PA-doped PBI membranes. Due to the high vacuum environment of conventional SEM, the beam-sensitivity of these membranes was reduced with a mild 120 C heat treatment to remove excess water without structural rearrangement (as verified from wide angle X-ray scattering). Cryo-SEM has also been implemented for both initial and heated membranes. Cryo-SEM is known to prevent dehydration of the specimen and reduce beam-sensitivity. The SEM cross-section image (Fig. 1A) of the heated samples exhibit 3{micro}m spheroidal features that are elongated in the direction of the casting blade. These features are distorted to 2{micro}m under conventional SEM conditions (Fig. 1B). The fine-scale gel morphology image (Fig. 2) is composed of 65nm diameter domains and 30nm walls, which resembles a cellular structure. In the future, the PA-doped PBI membranes will be cryo-microtomed and cryotransferred for elemental analysis in a TEM.
- Research Organization:
- Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Shared Research Equipment Collaborative Research Center
- Sponsoring Organization:
- USDOE Office of Energy Efficiency and Renewable Energy (EERE)
- DOE Contract Number:
- DE-AC05-00OR22725
- OSTI ID:
- 979171
- Resource Relation:
- Conference: Microscopy & Microanalysis 2009, Richmond, VA, USA, 20090726, 20090730
- Country of Publication:
- United States
- Language:
- English
Similar Records
A Comparative Study of Phosphoric Acid-doped m-PBI Membranes
Polybenzimidazole-Based Polymer Electrolyte Membranes for High-Temperature Fuel Cells: Current Status and Prospects