Direct Measurement of Microporosity and Molecular Accessibility in Stöber Spheres by Adsorption Isotherms

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Title: Direct Measurement of Microporosity and Molecular Accessibility in Stöber Spheres by Adsorption Isotherms
Authors: Farrando Pérez, Judit | López, Cefe | Silvestre-Albero, Joaquín | Gallego-Gómez, Francisco
Research Group/s: Materiales Avanzados
Center, Department or Service: Universidad de Alicante. Departamento de Química Inorgánica | Universidad de Alicante. Instituto Universitario de Materiales
Keywords: Microporosity | Molecular accessibility | Stöber spheres | Adsorption isotherms
Knowledge Area: Química Inorgánica
Issue Date: 5-Sep-2018
Publisher: American Chemical Society
Citation: The Journal of Physical Chemistry C. 2018, 122(38): 22008-22017. doi:10.1021/acs.jpcc.8b07278
Abstract: The microporous nature of monodisperse Stöber silica spheres is demonstrated in the literature, although usually via indirect evidence. Contradictorily, there also exist numerous reports of nonporosity based on conventional N2 adsorption isotherms, leading to a confusing scenario and questioning the evaluation methodology. Thus, there is the strong need of straight measure of microporosity in Stöber spheres, at best by available adsorption techniques, which must be further directly confronted with the standard nitrogen method. Here, for the first time, microporosity detection by N2 and CO2 adsorption is compared in Stöber spheres. We demonstrate that CO2 isotherms at 273 K allow direct detection and quantification of the microporosity (about 0.1 cm3/g in our samples), while N2 at 77 K cannot probe adequately the internal volume. We also show that a large amount of water fills the micropores under usual ambient conditions, also revealing the presence of small mesoporosity. Thus, the porous nature of Stöber spheres is investigated by a simple combination of adsorption isotherms, and the different accessibility of N2, CO2, and H2O molecules is discussed. We emphasize the inadequacy of standard N2 isotherms for micropore detection in Stöber silica, as the access of nitrogen molecules at cryogenic temperatures is kinetically restricted and may lead to erroneous conclusions. Instead, we propose CO2 isotherms as a simple and direct means for evaluation of microporosity.
Sponsor: This work was funded by Spanish MINECO Projects MAT2014-58731-JIN, MAT2015-68075-R, MAT2016-80285-p, and SIFE2; Comunidad de Madrid Projects S2013/MIT-2740 and PHAMA_2.0; Generalitat Valenciana Project PROMETEOII/2014/004, and Project EU H2020 MSCARISE-2016/NanoMed.
URI: http://hdl.handle.net/10045/81547
ISSN: 1932-7447 (Print) | 1932-7455 (Online)
DOI: 10.1021/acs.jpcc.8b07278
Language: eng
Type: info:eu-repo/semantics/article
Rights: © 2018 American Chemical Society
Peer Review: si
Publisher version: https://doi.org/10.1021/acs.jpcc.8b07278
Appears in Collections:INV - LMA - Artículos de Revistas
Research funded by the EU

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