Controversial reports regarding Stöber silica's microporosity and specific surface area remain in the literature despite decades of widespread applications. In this work, Stöber silica samples prepared under controlled reaction time and postsynthesis washing/drying conditions were characterized by nitrogen adsorption at 77 K, transmission electron microscopy, elemental analysis, Fourier transform infrared spectroscopy, thermal analysis, and evolved gas analysis. Our experimental results demonstrated the important but often overlooked effects of reaction time and postsynthesis treatments on Stöber silica's pore characteristics, as evidenced by the strikingly large range of BET specific surface area (11.3-309.7 m(2)/g). A simple micropore filling and blocking mechanism compatible with an existing Stöber silica growth model incorporating both aggregation and monomer addition steps was proposed to explain all our experimental findings. The carbon and nitrogen contents appear to serve well as the indicative link between our experimental variables and the resulting pore blocking by TEOS and its derivatives. A suitable combination of experimental conditions is recommended in order to make microporous Stöber silica samples with large specific surface area, including a short reaction time, water washing, and drying at moderate temperature preferably under vacuum.
Puzzling aspects of the microporous structure of Stöber silica, including inconsistencies in the BET specific surface area and the long measurement time required for N2 adsorption, hinder further research on and potential applications of this material. In this work, Stöber silica samples prepared using systematic and detailed post-treatment methods were characterized by N2 adsorption, scanning electron microscopy, transmission electron microscopy, inductively coupled plasma optical emission spectrometry, elemental analysis, and Fourier transform infrared spectroscopy. We have found that the often overlooked sample preparation conditions may be the main causes that perplex the gas adsorption characterization results of Stöber silica samples. The pore-blocking processes associated with a variety of sample treatment methods are discussed in detail. Strong evidence for the particle growth model and pore-blocking mechanism involving ethoxyl groups, Si species, and condensation of silanols is provided. A remarkable result is that the measurement time is shortened from 1 month in our previous work to 2-3 days for samples with large specific surface areas. A suitable post-treatment condition is recommended to obtain microporous Stöber silica with a short measurement time, including water washing, low temperature drying without a vacuum, and a short storage time.
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