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Title: Probing the Geometry and Interconnectivity of Pores in Organic Aerogels Using Hyperpolarized 129Xe NMR Spectroscopy

Journal Article · · Journal of the American Chemical Society, 126(16):5052-5053
DOI:https://doi.org/10.1021/ja049577x· OSTI ID:993674

Aerogels represent a class of novel open-pore materials with high surface area and nanometer pore sizes. They exhibit extremely low mass densities, low thermal conductivity, good acoustic insulation, and low dielectric constants. These materials have potential applications in catalysis, advanced separation techniques, energy storage, environmental remediation, and as insulating materials. Organic aerogels are stiffer and stronger than silica aerogels and are better insulators with higher thermal resistance. Resorcinol-Formaldehyde (RF) aerogels are typically prepared through the base-catalyzed sol-gel polymerization of resorcinol with formaldehyde in aqueous solution to produce gels, which are then dried in supercritical CO2.1,2 The [resorcinol]/ [catalyst] (R/C) ratio of the starting sol-gel solution has been determined to be the dominant factor that affects the properties of RF aerogels. Since the unique microstructures of aerogels are responsible for their unusual properties, characterizing the detailed porous structures and correlating them with the processing parameters are vital to establish rational design principles for novel organic aerogels with tailored properties. In this communication we report the first use of hyperpolarized (HP) 129Xe NMR to probe the geometry and interconnectivity of pores in RF aerogels and to correlate these with synthetic conditions. Our work demonstrates that HP 129Xe NMR is so far the only method for accurately measuring the free volume-to-surface-area (Vg/S) ratios for soft mesoporous materials without using any geometric models.

Research Organization:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Organization:
USDOE
DOE Contract Number:
AC05-76RL01830
OSTI ID:
993674
Report Number(s):
PNNL-SA-40666; JACSAT; KC0201050; TRN: US201023%%557
Journal Information:
Journal of the American Chemical Society, 126(16):5052-5053, Vol. 126, Issue 16; ISSN 0002-7863
Country of Publication:
United States
Language:
English