Highly microporous carbons with BET surface areas of up to ca. 3300 m2 g-1 and pore volumes of up to 1.6 cm3 g-1 have been successfully synthesized from pistachio shells, a waste whose generation is growing on account of the nutritive value of pistachios and the resilience of this crop to climate change. Such a high pore development has been achieved by a simple and benign CO2 physical activation process assisted by a custom pre-treatment of the biomass. Different approaches have been explored in this work for the transformation of pistachio shells into carbon materials with diverse microstructures, mineral matter content and particle size/morphology, tuning thereby their reactivities towards CO2 and diffusion kinetics and, in this way, pore development. In particular, the most efficient route for the production of highly microporous carbons from pistachio shells involves a hydrothermal carbonization process which increases the degree of aromatization and effectively removes the mineral matter, enhancing thereby the efficiency of both carbon production and porosity generation. By increasing the activation temperature, substantial shortening of the operation time can be achieved without compromising pore development. This work provides new integral strategies towards the production of biomass-based, CO2-activated carbons with a focus on optimizing pore structure, minimizing energy consumption and maximizing product yield., This research was supported by the European Commission, Horizon Europe Framework Program, Call HORIZON-CL4-2021-RESILIENCE-01, Project MAST3RBOOST, GA 101058574., Peer reviewed

Highly porous carbon microspheres have been obtained by a sustainable and facile approach that combines a microwave-assisted sol-gel process with a physical activation process. This approach is based on the use of sustainable monomers, such as phloroglucinol and glyoxylic acid, and CO2 as a benign activating agent. By implementing a microwave-assisted polymerization step, it was possible to reduce the aging time by >90 % compared to similar processes. In addition, a three-fold reduction in activation time was achieved by increasing the activation temperature but with no deleterious effects on textural properties or H2 storage capacity. In this way, carbon materials with BET surface area of up to 3300 m2 g−1 and pore volume of up to 1.6 cm3 g−1 were obtained, with >60 % of pore volume arising from micropores and with no pores larger than 3.5 nm. As a result, the carbons can store up to 9.2 wt% H2 at −196 °C and 100 bar with the H2 uptake mirroring trends in total porosity. Based on theoretical calculations, the working capacity could be enhanced by using a temperature pressure swing adsorption (TPSA) system (i.e., −196 °C, 100 bar to −123 °C, 5 bar) to 9.0 wt% H2, which is close to the total uptake at −196 °C and 100 bar. This compares to working capacity of 5.0 wt% H2 for a PSA system at −196 °C of 100 to 5 bar., This research was supported by the European Commission, Horizon Europe Framework Program, Call HORIZON-CL4-2021-RESILIENCE-01, Project MAST3RBOOST, GA 101058574., Peer reviewed

These data are associated with the published work: ChemSusChem 2025, 18, e202401288: From Green to Black Gold: Highly Microporous Carbons from Pistachio Shells by a Controlled Physical Activation Process, by Ana Fernández-Lera,[a] María Dolores Casal,[a] Quentin Judalet,[b] Noel Díez,[a]
Teresa Valdés-Solís,[a] and Marta Sevilla*[a], This research was supported by the European Commission, Horizon Europe Framework Program, Call HORIZON-CL4-2021-RESILIENCE-01, Project MAST3RBOOST, GA 101058574., Peer reviewed

These data are associated with the published work: Journal of Energy Storage 123 (2025) 116818: Sustainable and synthetic carbon polymers for safe and efficient H2 storage, by Ana Fernández-Lera [a], Maria Álvarez-Rodríguez [a], Maria Dolores Casal [a[], L. Scott Blankenship [b],
Robert Mokaya [b,c], Teresa Valdés-Solís [a], Ana Arenillas [a], Marta Sevilla [a]. [a] Instituto de Ciencia y Tecnología del Carbono (INCAR), CSIC, Oviedo, Spain; [b] School of Chemistry, University of Nottingham, Nottingham, United Kingdom; [c] School of Mathematical and Physical Sciences, University of Sheffield, United Kingdom, This research was supported by the European Commission, Horizon Europe Framework Program, Call HORIZON-CL4-2021-RESILIENCE-01, Project MAST3RBOOST, GA 101058574., Peer reviewed

Highly porous carbons with surface areas approaching 3300 m2 g−1 have been synthesized from eucalyptus sawdust and pistachio shells through controlled CO2 activation. The implementation of hydrothermal carbonization increases the global yield of the synthesis process and decreases the reactivity toward CO2 by decreasing the density of structural defects and removing virtually all the mineral matter contained in the residues. The last feature is a determining factor in porosity generation efficiency. Thereby, activation proceeds under chemical control, ensuring the uniform generation of porosity inside the particles, which leads to materials with relatively narrow pore size distributions in the micro-to small mesopore region (<3.5 nm). These materials store significant amounts of H2 at −196 °C/100 bar, reaching up to 9.8 wt%. Theoretical calculations show that the most energy-efficient way of storing H2 is using a TPSA system, which allows the working capacities to be substantially enhanced up to 9.7 wt%., This research was supported by the European Commission, Horizon Europe Framework Program, Call HORIZON-CL4-2021-RESILIENCE-01, Project MAST3RBOOST, GA 101058574., Peer reviewed

These data are associated with the published work: International Journal of Hydrogen Energy 254 (2026) 156367: Highly porous carbons from hydrochar by means of a controlled physical activation process and their hydrogen storage performance, by Ana Fernández-Lera[a], María Dolores Casal[a], Stephen Otieno [b], Leo Scott Blankenship [b], Robert Mokaya [b], Teresa Valdés-Solís[a] and Marta Sevilla*[a]. [a] Instituto de Ciencia y Tecnología del Carbono (INCAR), CSIC, Oviedo, Spain; [b] School of Chemistry, University of Nottingham, University Park, Nottingham, UK., This research was supported by the European Commission, Horizon Europe Framework Program, Call HORIZON-CL4-2021-RESILIENCE-01, Project MAST3RBOOST, GA 101058574., Peer reviewed