Microstructural control by freeze-casting of CaO architectures for improved and stable thermochemical energy storage performance

This study investigates the development of porous calcium-based monoliths via freeze-casting (FC) as a novel approach for thermochemical energy storage, particularly within the Calcium Looping (CaL) process. The freeze-casting technique enabled the fabrication of scaffolds with controlled porosity u...

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Autores: Amghar, Nabil, Ivorra-Martínez, Juan, Perejón, Antonio, Hanaor, Dorian, Gurlo, Aleksander, Ramírez-Rico, Joaquín, Pérez-Maqueda, Luis A., Sánchez-Jiménez, Pedro E.
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2025
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/393541
Acceso en línea:http://hdl.handle.net/10261/393541
https://api.elsevier.com/content/abstract/scopus_id/105004406062
Access Level:acceso abierto
Palabra clave:CaCO3
Calcium Looping
Freeze-casting
Porous structures
Thermochemical energy storage
http://metadata.un.org/sdg/13
Take urgent action to combat climate change and its impacts
energy
Energy conservation
id ES_c38cd3dda4d2aaa0e75ac713326ca7b3
oai_identifier_str oai:digital.csic.es:10261/393541
network_acronym_str ES
network_name_str España
repository_id_str
dc.title.none.fl_str_mv Microstructural control by freeze-casting of CaO architectures for improved and stable thermochemical energy storage performance
title Microstructural control by freeze-casting of CaO architectures for improved and stable thermochemical energy storage performance
spellingShingle Microstructural control by freeze-casting of CaO architectures for improved and stable thermochemical energy storage performance
Amghar, Nabil
CaCO3
Calcium Looping
Freeze-casting
Porous structures
Thermochemical energy storage
http://metadata.un.org/sdg/13
Take urgent action to combat climate change and its impacts
energy
Energy conservation
title_short Microstructural control by freeze-casting of CaO architectures for improved and stable thermochemical energy storage performance
title_full Microstructural control by freeze-casting of CaO architectures for improved and stable thermochemical energy storage performance
title_fullStr Microstructural control by freeze-casting of CaO architectures for improved and stable thermochemical energy storage performance
title_full_unstemmed Microstructural control by freeze-casting of CaO architectures for improved and stable thermochemical energy storage performance
title_sort Microstructural control by freeze-casting of CaO architectures for improved and stable thermochemical energy storage performance
dc.creator.none.fl_str_mv Amghar, Nabil
Ivorra-Martínez, Juan
Perejón, Antonio
Hanaor, Dorian
Gurlo, Aleksander
Ramírez-Rico, Joaquín
Pérez-Maqueda, Luis A.
Sánchez-Jiménez, Pedro E.
author Amghar, Nabil
author_facet Amghar, Nabil
Ivorra-Martínez, Juan
Perejón, Antonio
Hanaor, Dorian
Gurlo, Aleksander
Ramírez-Rico, Joaquín
Pérez-Maqueda, Luis A.
Sánchez-Jiménez, Pedro E.
author_role author
author2 Ivorra-Martínez, Juan
Perejón, Antonio
Hanaor, Dorian
Gurlo, Aleksander
Ramírez-Rico, Joaquín
Pérez-Maqueda, Luis A.
Sánchez-Jiménez, Pedro E.
author2_role author
author
author
author
author
author
author
dc.contributor.none.fl_str_mv European Commission
Ministerio de Ciencia e Innovación (España)
Ministerio de Ciencia, Innovación y Universidades (España)
European Science Foundation
Generalitat Valenciana
Universidad de Sevilla
Amghar, Nabil [0000-0002-0964-9899]
Ivorra-Martínez, Juan [0000-0001-8968-4899]
Perejón, Antonio [0000-0002-5525-2227]
Hanaor, Dorian [0000-0003-4455-7006]
Gurlo, Aleksander [0000-0001-7047-666X]
Ramírez-Rico, Joaquín [0000-0002-1184-0756]
Pérez-Maqueda, Luis A. [0000-0002-8267-3457]
Sánchez-Jiménez, Pedro E. [0000-0001-6982-1411]
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv CaCO3
Calcium Looping
Freeze-casting
Porous structures
Thermochemical energy storage
http://metadata.un.org/sdg/13
Take urgent action to combat climate change and its impacts
energy
Energy conservation
topic CaCO3
Calcium Looping
Freeze-casting
Porous structures
Thermochemical energy storage
http://metadata.un.org/sdg/13
Take urgent action to combat climate change and its impacts
energy
Energy conservation
description This study investigates the development of porous calcium-based monoliths via freeze-casting (FC) as a novel approach for thermochemical energy storage, particularly within the Calcium Looping (CaL) process. The freeze-casting technique enabled the fabrication of scaffolds with controlled porosity using polyvinyl alcohol (PVA) as a binder. Experimental results demonstrated that freeze-cast monoliths exhibited superior multicycle performance under various carbonation and calcination conditions. The FC-CaCO<inf>3</inf> monolith achieved the highest residual conversion of 68.1 % under mild vacuum calcination conditions (780 °C, 0.1 bar CO<inf>2</inf>), significantly surpassing other configurations. Tests conducted in an inert atmosphere also yielded favorable results, with a conversion of 56.1 %, outperforming equivalent raw powder samples. The enhanced performance is attributed to improved CO<inf>2</inf> interaction with the porous structure, mitigating sintering effects and preserving active surface area. Morphological observations by X-ray tomography and SEM confirmed limited particle sintering after multiple cycles, maintaining a reactive surface that supported consistent conversion rates. The pore size distribution of the material evolves upon cycling resulting in an increased microporosity, while the pore network maintains a low tortuosity (τ ~ 1.5–2.0). The addition of dopants such as ZrO<inf>2</inf> and SiO<inf>2</inf> did not enhance performance, as the monoliths' inherent structure provided sufficient stability. These findings highlight freeze-casting as a promising method for creating advanced porous materials suitable for energy storage applications.
publishDate 2025
dc.date.none.fl_str_mv 2025
2025
2025
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Publisher's version
info:eu-repo/semantics/publishedVersion
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/10261/393541
https://api.elsevier.com/content/abstract/scopus_id/105004406062
url http://hdl.handle.net/10261/393541
https://api.elsevier.com/content/abstract/scopus_id/105004406062
dc.language.none.fl_str_mv Inglés
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info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PDC2021-121552-C21
info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2021-2023/TED2021-131839B-C22
info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2021-2023/PID2022-140815OB-C22
CIAPOS/2023/362.
info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PRE2018-085866
https://doi.org/10.1016/j.est.2025.116681
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dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
dc.source.none.fl_str_mv reponame:DIGITAL.CSIC. Repositorio Institucional del CSIC
instname:Consejo Superior de Investigaciones Científicas (CSIC)
instname_str Consejo Superior de Investigaciones Científicas (CSIC)
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spelling Microstructural control by freeze-casting of CaO architectures for improved and stable thermochemical energy storage performanceAmghar, NabilIvorra-Martínez, JuanPerejón, AntonioHanaor, DorianGurlo, AleksanderRamírez-Rico, JoaquínPérez-Maqueda, Luis A.Sánchez-Jiménez, Pedro E.CaCO3Calcium LoopingFreeze-castingPorous structuresThermochemical energy storagehttp://metadata.un.org/sdg/13Take urgent action to combat climate change and its impactsenergyEnergy conservationThis study investigates the development of porous calcium-based monoliths via freeze-casting (FC) as a novel approach for thermochemical energy storage, particularly within the Calcium Looping (CaL) process. The freeze-casting technique enabled the fabrication of scaffolds with controlled porosity using polyvinyl alcohol (PVA) as a binder. Experimental results demonstrated that freeze-cast monoliths exhibited superior multicycle performance under various carbonation and calcination conditions. The FC-CaCO<inf>3</inf> monolith achieved the highest residual conversion of 68.1 % under mild vacuum calcination conditions (780 °C, 0.1 bar CO<inf>2</inf>), significantly surpassing other configurations. Tests conducted in an inert atmosphere also yielded favorable results, with a conversion of 56.1 %, outperforming equivalent raw powder samples. The enhanced performance is attributed to improved CO<inf>2</inf> interaction with the porous structure, mitigating sintering effects and preserving active surface area. Morphological observations by X-ray tomography and SEM confirmed limited particle sintering after multiple cycles, maintaining a reactive surface that supported consistent conversion rates. The pore size distribution of the material evolves upon cycling resulting in an increased microporosity, while the pore network maintains a low tortuosity (τ ~ 1.5–2.0). The addition of dopants such as ZrO<inf>2</inf> and SiO<inf>2</inf> did not enhance performance, as the monoliths' inherent structure provided sufficient stability. These findings highlight freeze-casting as a promising method for creating advanced porous materials suitable for energy storage applications.Financial support is acknowledged from grants TED2021-131839B-C22 and PDC2021-121552-C21 (MCIN/AEI/10.13039/501100011033 and European Union Next Generation EU/PRTR) and by European Union NextGenerationEU/PRTR, and the grant PID2022-140815OB-C22 funded by MCIN/AEI/10.13039/501100011033 and ERDF A way of making Europe. PhD Fellowship granted to N. Amghar (PRE2018-085866) from the Spanish Government Agency Ministerio de Ciencia, Innovación y Universidades. J. Ivorra-Martinez thanks Generalitat Valenciana - GVA for funding a postdoc position through the CIAPOS program co-funded by ESF Investing in your future, grant number CIAPOS/2023/362. XCT measurements were performed at the X-ray laboratory of the Research, Technology and Innovation Center (CITIUS) of the University of Seville.Peer reviewedElsevierEuropean CommissionMinisterio de Ciencia e Innovación (España)Ministerio de Ciencia, Innovación y Universidades (España)European Science FoundationGeneralitat ValencianaUniversidad de SevillaAmghar, Nabil [0000-0002-0964-9899]Ivorra-Martínez, Juan [0000-0001-8968-4899]Perejón, Antonio [0000-0002-5525-2227]Hanaor, Dorian [0000-0003-4455-7006]Gurlo, Aleksander [0000-0001-7047-666X]Ramírez-Rico, Joaquín [0000-0002-1184-0756]Pérez-Maqueda, Luis A. [0000-0002-8267-3457]Sánchez-Jiménez, Pedro E. [0000-0001-6982-1411]Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]202520252025info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501Publisher's versioninfo:eu-repo/semantics/publishedVersionapplication/pdfhttp://hdl.handle.net/10261/393541https://api.elsevier.com/content/abstract/scopus_id/105004406062reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Inglés#PLACEHOLDER_PARENT_METADATA_VALUE##PLACEHOLDER_PARENT_METADATA_VALUE##PLACEHOLDER_PARENT_METADATA_VALUE##PLACEHOLDER_PARENT_METADATA_VALUE##PLACEHOLDER_PARENT_METADATA_VALUE#info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PDC2021-121552-C21info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2021-2023/TED2021-131839B-C22info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2021-2023/PID2022-140815OB-C22CIAPOS/2023/362.info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PRE2018-085866https://doi.org/10.1016/j.est.2025.116681Síinfo:eu-repo/semantics/openAccessoai:digital.csic.es:10261/3935412026-05-22T06:33:51Z
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