Triangulation of pore structural characterisation of disordered mesoporous silica using novel hybrid methods involving dual-probe porosimetries

Mousa, Suleiman; Baron, Kyro; Fletcher, Robin S.; Rigby, Sean P.

Abstract

The key issue, in applying indirect pore structure characterisation methods to disordered materials, is that usually some physical assumptions are necessary to probe pore size, such as concerning the mode of the phase transition used, which determines meniscus geometry or kernel type. This issue often undermines the relative advantages of indirect methods, over direct methods like imaging, from both the wider range of pores sizes that can be probed in a single experiment and the much better statistical representativeness of the data, which are essential for highly heterogeneous disordered materials. Further, parameter calibrations provided using supposedly the same model ordered porous materials are often conflictual. However, this work introduces dual-liquid thermoporometry, and also dual-probe, serial water sorption and mercury intrusion, to complement multi-adsorbate, serial gas sorption, to overcome this issue by triangulating the data for three key probe molecules used in three different porosimetries, namely liquid intrusion, gas sorption, and thermoporometry. It has been found that augmenting one porosimetry, using just one probe molecule, to a dual-probe experiment removes the aforementioned, key drawback of indirect methods. The alternative, complementary dual-probe porosimetries can also cross-validate this approach for each other. This allows indirect methods to stand alone, without the need for direct imaging methods to inform or validate prior assumptions. Further, the dual-probe experiments allow additional information on pore structure to be obtained beyond that provided by single-probe experiments. For example, dual-liquid thermoporometry also allows the probing for the presence and nature of the advanced melting effect, and serial water adsorption and mercury porosimetry delivers information on network filling mechanisms during adsorption in disordered media.

Citation

Mousa, S., Baron, K., Fletcher, R. S., & Rigby, S. P. (2022). Triangulation of pore structural characterisation of disordered mesoporous silica using novel hybrid methods involving dual-probe porosimetries. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 653, Article 130026. https://doi.org/10.1016/j.colsurfa.2022.130026

• Journal Article Type: Article
• Acceptance Date: Aug 20, 2022
• Online Publication Date: Aug 24, 2022
• Publication Date: Nov 20, 2022
• Deposit Date: Aug 25, 2022
• Publicly Available Date: Aug 25, 2023
• Journal: Colloids and Surfaces A: Physicochemical and Engineering Aspects
• Print ISSN: 0927-7757
• Electronic ISSN: 1873-4359
• Publisher: Elsevier BV
• Peer Reviewed: Peer Reviewed
• Volume: 653
• Article Number: 130026
• DOI: https://doi.org/10.1016/j.colsurfa.2022.130026
• Keywords: Colloid and Surface Chemistry
• Public URL: https://nottingham-repository.worktribe.com/output/10364488
• Publisher URL: https://www.sciencedirect.com/science/article/pii/S0927775722017812