Advanced and delayed filling or emptying of pore entities by vapor sorption or liquid intrusion in simulated porous networks

Matadamas, Jorge; Alférez, Reyna; López, Ramírez; Román, G.; Kornhauser, Isaac; Rojas, Fernando

doi:10.1016/j.colsurfa.2015.09.072

Cited by 9 publications

(12 citation statements)

References 21 publications

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“…pore-pore interaction) delayed condensation effect using integrated porosimetry experiments 14 . This effect has been shown, from simulations on model pore networks, to greatly impact the accuracy of gas sorption pore size distributions 28 .…”

Section: Introductionmentioning

confidence: 99%

“…The difference in the wetting of mercury by argon and nitrogen has been used to detect the network-based (i.e., pore–pore interaction) delayed condensation effect using integrated porosimetry experiments . This effect has been shown, from simulations on model pore networks, to greatly impact the accuracy of gas sorption pore size distributions …”

Section: Introductionmentioning

confidence: 99%

“…14 This effect has been shown, from simulations on model pore networks, to greatly impact the accuracy of gas sorption pore size distributions. 28 It is the purpose of this work to utilize the different wetting toward mercury surfaces by argon and nitrogen to probe pore size interconnectivity. The tendency for mercury to become entrapped in the largest pores 29 means that mercury can be used to preferentially fill particular subsets of the pore size distribution, such as macroporous "highways" (or "motorways").…”

Section: Introductionmentioning

confidence: 99%

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Determination of Pore Network Accessibility in Hierarchical Porous Solids

Rigby

Hasan

Stevens

et al. 2017

Ind. Eng. Chem. Res.

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This paper validates the hypothesis that the supposedly non-specific adsorbates nitrogen and argon wet heavy metals differently, and shows how this unexpected effect can be actively utilised to deliver information on pore inter-connectivity. To explore surface chemistry influences on differential adsorbate wetting, new findings for a mixed silica-alumina material were compared with data for pure silica and alumina materials. The new structural characterisation described can determine the distribution of the particular sub-set of mesoand micro-pores that connect directly to macropores that entrap mercury following porosimetry, as mapped by computerised X-ray tomography. Hence, it elucidates the spatial organization of the network and measures the improved accessibility to smaller pores provided by larger pores. It was shown that the silica-alumina pellets have a hierarchical pore-size arrangement, similar to the optimal blood vessel network architecture in animals.The network architecture derived from the new method has been independently validated using complementary gas sorption scanning curves, integrated mercury porosimetry, and NMR cryoporometry. It has also been shown that, rather than hindering interpretation of characterisation data, emergent effects for networks associated with these techniques can be marshalled to enable detailed assessment of the pore structures of complex, disordered solids. Keywords: adsorbate; wetting; pore network; connectivity; co-operative effects; imaging Recently, hierarchical porous solids have become of particular interest for various applications [3][4][5][6][7][8] . Computer simulations can predict the likely relative performance of the various potential network architectures 9,10 . A common design proposed to overcome diffusion limitations includes pore networks similar to the tree-like arrangement of passages within the human lung, whereby macropores provide rapid access to the interior, and steadily smaller pores ('lanes') leading off these 'highways' to provide higher surface area for reaction.Various degrees of structural control are possible, depending upon the sophistication, and thence cost, of the synthesis method for the material. Even surfactant-templated materials may contain regions of disorder 1 . Hence, for quality control, the uniformity of manufactured product must be validated to ensure it all has the desired structure. Further, in some reactions the void space of the catalyst pellet may evolve over time due to solids deposition, as in coking 5 . It is thus essential to be able to characterise the spatial arrangement of the various pore sizes, arising from the distribution, as they are juxtaposed relative to each other.Modern imaging techniques, such as electron tomography (or 3D transmission electron microscopy (TEM)) 12 , dual-beam scanning electron microscopy (SEM) (or focused ion-beam SEM) 13,14 , and computerised X-ray tomography (CXT or CT) 15 , can provide full threedimensional reconstructions of the void space of mesoporous materials at nanometre re...

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Determination of Pore Network Accessibility in Hierarchical Porous Solids

Rigby

Hasan

Stevens

et al. 2017

Ind. Eng. Chem. Res.

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“…The potential impact of the co-operative phenomena on PSD accuracy has been demonstrated by computer simulation of adsorption in pore network models [7]. Matadamas et al [7] have simulated the effects of delayed and advanced adsorption in pore body-pore neck network models with a range of pore connectivities, and overlaps between pore body and neck size distributions.…”

Section: Introductionmentioning

confidence: 99%

“…Matadamas et al [7] have simulated the effects of delayed and advanced adsorption in pore body-pore neck network models with a range of pore connectivities, and overlaps between pore body and neck size distributions. They compared the actual pore space characteristics of the underlying models with those obtained, by standard analysis methods, from the simulated isotherms, and showed that delayed condensation gave rise to a significant error in the accuracy of the PSD derived.…”

Section: Introductionmentioning

confidence: 99%

Detection of the delayed condensation effect and determination of its impact on the accuracy of gas adsorption pore size distributions

Rigby

Hasan

Hitchcock

et al. 2017

Colloids and Surfaces A: Physicochemical and Engineering Aspect

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The version presented here may differ from the published version or from the version of record. If you wish to cite this item you are advised to consult the publisher's version. Please see the repository url above for details on accessing the published version and note that access may require a subscription.For more information, please contact eprints@nottingham.ac.uk 1 normally requiring assumptions about the correct model for data analysis. In this work we present a novel method to both expand the range, and obtain greater accuracy, for the information obtained from the main boundary adsorption isotherms by using a combination of data obtained for two adsorptives, namely nitrogen and argon, both before and after mercury porosimetry. The method makes use of the fact that nitrogen and argon apparently 'see' a different pore geometry following mercury entrapment, with argon, relatively, 'ignoring' new metal surfaces produced by mercury porosimetry. The new method permits the study of network and pore-pore co-operative effects during adsorption that substantially affect the accuracy of the characteristic parameters, such as modal pore size, obtained for disordered materials. These effects have been explicitly quantified, for a typical sol-gel silica catalyst support material as a case study. The technique allowed the large discrepancies between modal pore sizes obtained from standard gas adsorption and mercury thermoporometry methods to be attributed to the network-based delayed condensation effect, rather than spinodal adsorption. Once the network-based delayed condensation effect had been accounted for, the simple cylindrical pore model and macroscopic thermodynamic Kelvin-Cohan equation were then found sufficient to accurately describe adsorption in the material studied, rather than needing a more complex microscopic theory. Hence, for disordered mesoporous solids, a proper account of inter-pore interactions is more important than that of intra-pore adsorbate density distribution, to obtain accurate pore size distributions. Detection of the Delayed Condensation Effect and Determination of its

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Gas Sorption

Rigby

2020

Structural Characterisation of Natural and Industrial Porous Materials: A Manual

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Advanced and delayed filling or emptying of pore entities by vapor sorption or liquid intrusion in simulated porous networks

Cited by 9 publications

References 21 publications

Determination of Pore Network Accessibility in Hierarchical Porous Solids

Determination of Pore Network Accessibility in Hierarchical Porous Solids

Detection of the delayed condensation effect and determination of its impact on the accuracy of gas adsorption pore size distributions

Gas Sorption

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