Microporosity Quantification via NMR Relaxometry

[EN] Micropores and their interplay with liquids are critical in many solid systems but challenging to investigate, often requiring complex and indirect techniques to even be detected. Here, we perform low-field H NMR transverse relaxometry on submicron Stöber silica spheres to directly detect micro...

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Detalles Bibliográficos
Autores: Gallego-Gómez, Francisco, Cadar, Calin, López, Cefe, Ardelean, Ioan
Tipo de recurso: artículo
Estado:Versión aceptada para publicación
Fecha de publicación:2019
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/227325
Acceso en línea:http://hdl.handle.net/10261/227325
Access Level:acceso abierto
Palabra clave:NMR relaxometry
Microporosity
Liquids
Descripción
Sumario:[EN] Micropores and their interplay with liquids are critical in many solid systems but challenging to investigate, often requiring complex and indirect techniques to even be detected. Here, we perform low-field H NMR transverse relaxometry on submicron Stöber silica spheres to directly detect micropore water. Colloidal crystals with a well-defined sphere configuration are used to facilitate unambiguous distinction of the interparticle void water and enable straightforward micropore volume quantification. We evidence significant microporosity (∼16% of the sphere volume) with high water accessibility and monitor the drying of the micropore water, which exhibits high resilience, evaporating only after complete void drainage. Progressive microporosity closure by thermal annealing above 600 °C is shown, until complete removal at 900 °C. Increasing hydrophobicity of the micropore walls is observed, although it barely affected the water access. Our results prove the capability of NMR relaxometry to quantitatively investigate complex microporosity and the behavior of water confined therein.