Person: Lafuente Adiego, Marta
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Lafuente Adiego
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Marta
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Ciencias
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Publication Open Access In situ synthesis of SERS-active Au@POM nanostructures in a microfluidic device for real-time detection of water pollutants(American Chemical Society, 2020) Lafuente Adiego, Marta; Pellejero, Ismael; Clemente, Alberto; Urbiztondo, Miguel A.; Mallada, Reyes; Reinoso, Santiago; Pina, María P.; Gandía Pascual, Luis; Institute for Advanced Materials and Mathematics - INAMAT2; Gobierno de Navarra / Nafarroako Gobernua; Universidad Pública de Navarra / Nafarroako Unibertsitate PublikoaWe present a simple, versatile and low-cost approach for the preparation of SERS-active regions within a microfluidic channel 50 cm in length. The approach involves the UV-light-driven formation of polyoxometalate-decorated gold nanostructures, Au@POM (POM: H3PW12O40 (PW) and H3PMo12O40 (PMo)), that self-assemble in situ on the surface of the PDMS microchannels without any extra functionalization procedure. The fabricated LoCs were characterized by SEM, UV-Vis, Raman, XRD and XPS techniques. The SERS activity of the resulting Au@POM–coated lab-on-a-chip (LoC) devices was evaluated in both static and flow conditions using Rhodamine R6G. The SERS response of Au@PW–based LoCs was found superior to Au@PMo counterparts and outstanding when compared to reported data on metal@POM nanocomposites. We demonstrate the potentialities of both Au@POM–coated LoCs as analytical platforms for real time detection of the organophosphorous pesticide Paraoxon-methyl at 10-6 M concentration level.Publication Open Access Highly sensitive SERS quantification of organophosphorous chemical warfare agents: a major step towards the real time sensing in the gas phase(Elsevier, 2018) Lafuente Adiego, Marta; Pellejero, Ismael; Sebastián, Víctor; Urbiztondo, Miguel A.; Mallada, Reyes; Institute for Advanced Materials and Mathematics - INAMAT2A surface-enhanced Raman scattering (SERS)-based sensor was developed for the label-free real-time gas phase detection of dimethyl methylphosphonate (DMMP); a surrogate molecule of the G-series nerve agents which are of particular concern due to its extreme toxicity, persistence and previous deployment. The SERS platform was designed using simple elements (Au nano-particles) coated with a citrate layer, and a self-assembly procedure that yields near- optimum distances among the nanoparticles. The citrate coating acts as an effective trap of the target molecules on the immediate vicinity of the Au nanoparticle surface under ambient conditions by reversible hydrogen bonding type interactions. For the first time, we have been able to detect sub-ppm concentrations of DMMP in gas phase (130 parts-per-billion), as might be found on potential emergency scenarios. The high sensitivity, simple preparation and reusability of the SERS platforms developed in this work open up the way for immediate detection of chemical warfare agents in realistic scenarios.Publication Open Access Highly selective CO formation via CO2 hydrogenation over novel ceria-based high-entropy oxides (HEOs)(Elsevier, 2025-03-01) Cortázar, María; Lafuente Adiego, Marta; Navarro Puyuelo, Andrea; García, Xènia; Llorca, Jordi; Reyero Zaragoza, Inés; Bimbela Serrano, Fernando; Gandía Pascual, Luis; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Universidad Pública de Navarra / Nafarroako Unibertsitate PublikoaIn the present study, new ceria-based high-entropy oxides (HEOs) were investigated as CO2 hydrogenation catalysts. The nominal composition was (Ce0.5Ni0.1Co0.1Cu0.1Zn0.1Mg0.1)Ox and the synthesis was accomplished through the citrate complexing sol-gel method. Characterization techniques utilized including ICP-AES, in situ XRD and in situ XPS, SEM-EDS, HR-TEM and HAADF-STEM, Raman spectroscopy, H2-TPR, CO2-TPD and N2 physical adsorption. The physicochemical characterization and the catalytic results revealed that the conditions of the thermal treatments at which the oxides were subjected critically determined the catalytic performance, especially the CO2 hydrogenation products selectivities. Calcination in air and/or reduction in hydrogen conducted at temperatures below 500 °C led to active but poorly selective catalysts that produced both methane and CO with significant yields. This was mainly attributed to the presence of metallic Cu, Ni and Co on the catalysts that appeared to be supported on ceria doped with the rest of the formulation elements. In contrast, thermal treatments at 750 °C favored the formation of a rocksalt entropy-stabilized (NiCoCuZnMg)Ox HEO supported on ceria that has stood out for showing an excellent selectivity towards the reverse water¿gas shift (RWGS) reaction. This catalyst led to CO selectivities of almost 100 % over a very wide range of reaction temperatures (300-700 °C). Long-term stability tests (100 h) showed only a slight decrease in CO2 conversion, while CO selectivity remained stable at nearly 100 % at 400 °C. XRD characterization of the used catalysts evidenced that, whereas the basic catalyst structure remained, some metallic copper exsolved during reduction and reaction period. These results are relevant and very promising, opening a door to the development of new catalysts for the valorization of CO2 through the RWGS reaction, thus expanding the low-temperature limit at which this process can be carried out selectively.Publication Open Access Wettability control on microstructured polypropylene surfaces by means of O2 plasma(Wiley, 2017) Lafuente Adiego, Marta; Martínez, Elena; Pellejero, Ismael; Artal, María del Carmen; Pina, María del Pilar; Institute for Advanced Materials and Mathematics - INAMAT2Durable and wear resistant polypropylene surfaces with static contact angle (SCA) above 140° have been fabricated using standard photolithographic process and O2 plasma etching followed by thermal annealing at 100 °C. This microfabrication process leads to a hierarchical topography derived from the patterned microstructures and the sub‐micron roughness caused by plasma. Hydrophobicity (SCA up to 145°) remained over 14 months after fabrication. This wetting behavior is attributed to the combination of the periodic array of micro‐sized pillars with low aspect‐ratio and the submicron roughness caused by O2 plasma.Publication Open Access UiO-66 MOF-Derived Ru@ZrO2 catalysts for photo-thermal CO2 hydrogenation(MDPI, 2023) Almazán, Fernando; Lafuente Adiego, Marta; Echarte Villeras, Amaya; Imizcoz Aramburu, Mikel; Pellejero, Ismael; Gandía Pascual, Luis; Institute for Advanced Materials and Mathematics - INAMAT2; Universidad Pública de Navarra / Nafarroako Unibertsitate PublikoaThe use of metal–organic frameworks (MOFs) as templates or precursors in the manufacture of heterogeneous catalysts is highly attractive due to the transfer of MOFs’ inherent porosity and homogeneous metallic distribution to the derived structure. Herein, we report on the preparation of MOF-derived Ru@ZrO2 catalysts by controlled thermal treatment of zirconium-based MOF UiO66 with ruthenium moieties. Ru3+ (3 or 10 mol%) precursor was added to UiO-66 synthesis and, subsequently, the as-synthesized hybrid structure was calcined in flowing air at different temperatures (400–600 ◦C) to obtain ZrO2 -derived oxides doped with highly dispersed Ru metallic clusters. The materials were tested for the catalytic photo-thermal conversion of CO2 to CH4 . Methanation experiments were conducted in a continuous flow (feed flow rate of 5 sccm and 1:4 CO2 to H2 molar ratio) reactor at temperatures from 80 to 300 ◦C. Ru0.10@ZrO2 catalyst calcined at 600 ◦C was able to hydrogenate CO2 to CH4 with production rates up to 65 mmolCH4·gcat. –1 ·h –1, CH4 yield of 80% and nearly 100% selectivity at 300 ◦C. The effect of the illumination was investigated with this catalyst using a high-power visible LED. A CO2 conversion enhancement from 18% to 38% was measured when 24 sun of visible LED radiation was applied, mainly due to the increase in the temperature as a result of the efficient absorption of the radiation received. MOF-derived Ru@ZrO2 catalysts have resulted to be noticeably active materials for the photo-thermal hydrogenation of CO2 for the purpose of the production of carbon-neutral methane. A remarkable effect of the ZrO2 crystalline phase on the CH4 selectivity has been found, with monoclinic zirconia being much more selective to CH4 than its cubic allotrope.