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Beyond the Meso/Macroporous Boundary: Extending Capillary Condensation-Based Pore Size Characterization in Thin Films Through Tailored Adsorptives.

ABSTRACT: The characterization of thin films containing nanopores with diameters exceeding 50 nm poses significant challenges, especially when deploying sorption-based techniques. Conventional volumetric physisorption or mercury intrusion methods have limited applicability in thin films due to constraints in sample preparation and nondestructive testing. In this context, ellipsometric porosimetry represents a viable alternative, leveraging its optical sensitivity to thin films. With existing setups relying on the capillary condensation of volatile compounds such as water, applicability is typically restricted to pore dimensions <50 nm. In this study, we introduce two high-molar-mass hydrocarbon adsorptives, namely ethylbenzene and n-nonane. These adsorptives exhibit substantial potential in improving the accuracy of physisorption measurements beyond mesoporosity (i.e., >50 nm). Specifically, with n-nonane, applicability is extended up to 80 nm pores. Our measurement guidelines propose a nondestructive, expeditious (<60 min), low-pressure (<0.03 bar) approach to investigate nanoporous thin films with potential adaptability to diverse structural architectures.

SUBMITTER: Furedi M

PROVIDER: S-EPMC10860133 | biostudies-literature | 2024 Feb

REPOSITORIES: biostudies-literature

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Beyond the Meso/Macroporous Boundary: Extending Capillary Condensation-Based Pore Size Characterization in Thin Films Through Tailored Adsorptives.

Füredi Máté M Manzano Cristina V CV Marton András A Fodor Bálint B Alvarez-Fernandez Alberto A Guldin Stefan S

The journal of physical chemistry letters 20240130 5

The characterization of thin films containing nanopores with diameters exceeding 50 nm poses significant challenges, especially when deploying sorption-based techniques. Conventional volumetric physisorption or mercury intrusion methods have limited applicability in thin films due to constraints in sample preparation and nondestructive testing. In this context, ellipsometric porosimetry represents a viable alternative, leveraging its optical sensitivity to thin films. With existing setups relyin ...[more]

PMID: 38290522

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Project description:Arsenic pollution in ground and drinking water is a major problem worldwide due to the natural abundance of arsenic by dissolution from ground sediment or mining activities from anthropogenic activities. To overcome this issue, iron oxides as low-cost and non-toxic materials, have been widely studied as efficient adsorbents for arsenic removal, including when dispersed within porous silica supports. In this study, two head-to-head comparisons were developed to highlight the As(v)-adsorptive ability of meso- and macrostructured silica-based adsorbents. First, the role of the textural properties of a meso-(SBA15) and macrostructured (MOSF) silica support in affecting the structural-morphological features and the adsorption capacity of the active phase (Fe2O3) have been studied. Secondly, a comparison of the arsenic removal ability of inorganic (Fe2O3) and organic (amino groups) active phases was carried out on SBA15. Finally, since silica supports are commonly proposed for both environmental and biomedical applications as active phase carriers, we have investigated secondary silicon and iron pollution. The batch tests at different pH revealed better performance from both Fe2O3-composites at pH 3. The values of q m of 7.9 mg g-1 (53 mg gact -1) and 5.5 mg g-1 (37 mg gact -1) were obtained for SBA15 and MOSF, respectively (gact stands for mass of the active phase). The results suggest that mesostructured materials are more suitable for dispersing active phases as adsorbents for water treatment, due to the obtainment of very small Fe2O3 NPs (about 5 nm). Besides studying the influence of the pore size of SBA15 and MOSF on the adsorption process, the impact of the functionalization was analyzed on SBA15 as the most promising sample for As(v)-removal. The amino-functionalized SBA15 adsorbent (3-aminopropyltriethoxysilane, APTES) exhibited a q m of 12.4 mg g-1 and faster kinetics. Furthermore, issues associated with the release of iron and silicon during the sorption process, causing secondary pollution, were evaluated and critically discussed.

Dataset Information

Beyond the Meso/Macroporous Boundary: Extending Capillary Condensation-Based Pore Size Characterization in Thin Films Through Tailored Adsorptives.

Publications

Beyond the Meso/Macroporous Boundary: Extending Capillary Condensation-Based Pore Size Characterization in Thin Films Through Tailored Adsorptives.

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