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Title: Microporous silica prepared by organic templating: Relationship between the molecular template and pore structure

Journal Article · · Chemistry of Materials
DOI:https://doi.org/10.1021/cm980517y· OSTI ID:351552
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  1. Univ. of New Mexico, Albuquerque, NM (United States)

Microporous silica materials with a controlled pore size and a narrow pore size distribution have been prepared by sol-gel processing using an organic-templating approach. Microporous networks were formed by pyrolytic removal of organic ligands (methacryloxypropyl groups) from organic/inorganic hybrid materials synthesized by copolymerization of 3-methacryloxypropylsilane (MPS) and tetraethoxysilane (TEOS). Molecular simulations and experimental measurements were conducted to examine the relationship between the microstructural characteristics of the porous silica (e.g., pore size, total pore volume, and pore connectivity) and the size and amount of organic template ligands added. Adsorption measurements suggest that the final porosity of the microporous silica is due to both primary pores (those present in the hybrid material prior to pyrolysis) and secondary pores (those created by pyrolytic removal of organic templates). Primary pores were inaccessible to N{sub 2} at 77 K but accessible to CO{sub 2} at 195 K; secondary pores were accessible to both N{sub 2} (at 77 K) and CO{sub 2} (at 195 K) in adsorption measurements. Primary porosity decreases with the amount of organic ligands added because of the enhanced densification of MPS/TEOS hybrid materials as the mole fraction of trifunctional MPS moieties increases. Pore volumes measured by nitrogen adsorption experiments at 77 K suggest that the secondary (template-derived) porosity exhibits a percolation behavior as the template concentration is increased. Gas permeation experiments indicate that the secondary pores are approximately 5 {angstrom} in diameter, consistent with predictions based on molecular simulations.

Research Organization:
Sandia National Laboratories (SNL), Albuquerque, NM, and Livermore, CA (United States)
Sponsoring Organization:
USDOE, Washington, DC (United States); New Mexico Univ., Albuquerque, NM (United States); Electric Power Research Inst., Palo Alto, CA (United States); National Science Foundation, Washington, DC (United States)
DOE Contract Number:
AC04-94AL85000
OSTI ID:
351552
Journal Information:
Chemistry of Materials, Vol. 11, Issue 5; Other Information: PBD: May 1999
Country of Publication:
United States
Language:
English