Reinoso, Santiago
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Reinoso
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Santiago
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InaMat2. Instituto de Investigación en Materiales Avanzados y Matemáticas
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Publication Open Access From fundamental materials chemistry to sensing applications: unravelling the water adsorption mechanism of a luminescent optical fibre sensor membrane(Elsevier, 2024) Cruz Quesada, Guillermo; Rosales Reina, María Beatriz; López Torres, Diego; Reinoso, Santiago; López Ramón, María Victoria; Arzamendi Manterola, Gurutze; Elosúa Aguado, César; Espinal Viguri, Maialen; Garrido Segovia, Julián José; Ciencias; Ingeniería Eléctrica, Electrónica y de Comunicación; Institute for Advanced Materials and Mathematics - INAMAT2; Institute of Smart Cities - ISC; Zientziak; Ingeniaritza Elektrikoa, Elektronikoaren eta Telekomunikazio Ingeniaritzaren; Universidad Pública de Navarra / Nafarroako Unibertsitate PublikoaThis work provides insight into the correlation between the luminescent response of a water-vapour optical fibre sensor and the textural properties of its lanthanide-doped silica coating. To this end, a library of 16 silica xerogels derived from combinations between 2 lanthanide dopants (EuIII, TbIII) and 8 antenna ligands was synthesised and characterised by photoluminescence spectroscopy and N2 and CO2 adsorption-desorption isotherms, among others. Based on the best luminescent response and most-suited porous texture, the material doped with TbIII and 2,2′-(4-(2-Ethoxyethoxy)pyridine-2,6-diyl)bis(4,5-dihydrooxazole) was selected to construct the probe. A film of this material was affixed to a commercial silica fibre by dip-coating and the resulting sensor was tested in a climatic chamber with relative humidity ranging from 20 to 90% to obtain normalised time-response and calibration curves at three temperatures. The response was linear up to certain water-vapour concentrations, beyond which abruptly changed to polynomial, acting against the sensor resolution. The adsorption mechanism was elucidated by comparing the isosteric enthalpies of adsorption calculated from the sensor calibration curves to those determined from the monolith water-vapour isotherms, revealing that capillary condensation in the membrane mesopores was the key phenomenon leading to the response deviating from linearity.Publication Open Access Tuning the sensitivity of photonic sensors toward alkanes through the textural properties of hybrid xerogel coatings(Wiley, 2025-01-15) Rosales Reina, María Beatriz; López Torres, Diego; Cruz Quesada, Guillermo; Espinal Viguri, Maialen; Elosúa Aguado, César; Reinoso, Santiago; Garrido Segovia, Julián José; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ingeniería Eléctrica, Electrónica y de Comunicación; Ingeniaritza Elektrikoa, Elektronikoa eta Telekomunikazio Ingeniaritza; Institute of Smart Cities - ISC; Universidad Pública de Navarra / Nafarroako Unibertsitate PublikoaThis work exemplifies how incorporating organosilane modifiers into silica matrices allows for tuning the optical response of reflection photonic sensors through customizing the textural properties of hybrid xerogel sensing films. Xerogels with propyl molar percentages 0, 5, and 10% are used to construct photonic probes (OFS0pTEOS, OFS5pTEOS and OFS10pTEOS, respectively) by dip-coating upon optimizing film deposition parameters. The time response of these probes toward a battery of volatile organic compounds (VOCs) comprising species with different functionality, size-shape, and polarity is systematically analyzed through ON/OFF experiments, revealing that a low propyl content makes the poor-responding OFS0pTEOS film highly sensitive toward non-aromatic, large molecules with low-polar or non-polar character in OFS5pTEOS. This sensor is particularly sensitive toward alkanes, with globular cyclohexane (cyHex) outperforming elongated n-hexane. Variable-temperature calibration curves obtained from step-by-step experiments and adsorption-desorption cycles corroborate these observations and allow hysteresis to be quantified. The response to cyHex closely follows VOC concentration changes with the most stable signal among analytes, leading to well-defined curves with low-to-negligible hysteresis. The isosteric enthalpies of cyHex adsorption are obtained for both the bulk material and the sensor, demonstrating labile adsorbate-adsorbent interactions ruling the sensor response and becoming more exothermic for larger VOC concentrations.