Controlled Synthesis of Nickel Phosphides in Hollow N, P Co-Doped Carbon: In Situ Transition to (Oxy)hydroxide Phases During Oxygen Evolution Reaction

Developing sustainable and efficient electrocatalysts for the oxygen evolution reaction (OER) is crucial for advancing energy storage technologies. This study explored the dual role of phosphorus as a dopant in carbon matrices and a key component in nickel phosphides (Ni<inf>2</inf>P and...

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Authors: Ríos Ruiz, D., Arévalo Cid, Pablo, Cebollada Borao, Jesús, Celorrio, V., Haeussler, M., Drev, S., Martínez Huerta, M. Victoria
Format: article
Status:Published version
Publication Date:2025
Country:España
Institution:Consejo Superior de Investigaciones Científicas (CSIC)
Repository:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/419754
Online Access:http://hdl.handle.net/10261/419754
https://www.scopus.com/inward/record.uri?eid=2-s2.0-105001271300&doi=10.3390%2Fcatal15030292&partnerID=40&md5=11c89e4119373391cd68e2e968acc4a2
Access Level:Open access
Keyword:co-doped carbon
electrocatalyst
hollow nanostructures
nickel phosphide
oxygen evolution reaction
polydopamine
solvothermal method
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spelling Controlled Synthesis of Nickel Phosphides in Hollow N, P Co-Doped Carbon: In Situ Transition to (Oxy)hydroxide Phases During Oxygen Evolution ReactionRíos Ruiz, D.Arévalo Cid, PabloCebollada Borao, JesúsCelorrio, V.Haeussler, M.Drev, S.Martínez Huerta, M. Victoriaco-doped carbonelectrocatalysthollow nanostructuresnickel phosphideoxygen evolution reactionpolydopaminesolvothermal methodDeveloping sustainable and efficient electrocatalysts for the oxygen evolution reaction (OER) is crucial for advancing energy storage technologies. This study explored the dual role of phosphorus as a dopant in carbon matrices and a key component in nickel phosphides (Ni<inf>2</inf>P and Ni<inf>12</inf>P<inf>5</inf>), synthesized using dopamine (PDA) and ammonium phosphate as eco-friendly precursors. The phase formation of nickel phosphides was found to be highly dependent on the P/PDA ratio (0.15, 0.3, 0.6, and 0.9), allowing for the selective synthesis of Ni<inf>2</inf>P or Ni<inf>12</inf>P<inf>5</inf>. Operando Raman spectroscopy revealed that both phases undergo surface transformation into nickel (oxy)hydroxide species under OER conditions, yet Ni<inf>2</inf>P-based catalysts demonstrated superior activity and long-term stability. This enhancement is attributed to efficient electron transfer at the dynamic Ni<inf>2</inf>P/NiOOH interface. Additionally, hollow nanostructures formed at intermediate P/PDA ratios (≤0.3) via the Kirkendall effect and Ostwald ripening contributed to an increased specific surface area and micropore volume, further improving the catalytic performance. Electrochemical impedance spectroscopy confirmed reduced interfacial resistance and enhanced charge transport. These findings offer new insights into the rational design of high-performance electrocatalysts and propose a green, tunable synthesis approach for advanced energy conversion applications. © 2025 by the authors.This research was funded by the Comunidad de Madrid, Y2020/EMT-6419 “CEOTRES” project and by the MCIN/AEI/10.13039/501100011033, TED2021-129694B-C22 “DEFY-CO2” project. The authors gratefully acknowledge the funding from the European Union’s Horizon 2020 research and innovation programme under grant agreement No. 823717–ESTEEM3.Peer reviewedMultidisciplinary Digital Publishing InstituteComunidad de MadridAgencia Estatal de Investigación (España)Ministerio de Ciencia e Innovación (España)Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]202620262025info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501Publisher's versioninfo:eu-repo/semantics/publishedVersionhttp://hdl.handle.net/10261/419754https://www.scopus.com/inward/record.uri?eid=2-s2.0-105001271300&doi=10.3390%2Fcatal15030292&partnerID=40&md5=11c89e4119373391cd68e2e968acc4a2reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Inglés#PLACEHOLDER_PARENT_METADATA_VALUE#info:eu-repo/grantAgreement///Catalystshttps://doi.org/10.3390/catal15030292Síinfo:eu-repo/semantics/openAccessoai:digital.csic.es:10261/4197542026-05-22T06:33:51Z
dc.title.none.fl_str_mv Controlled Synthesis of Nickel Phosphides in Hollow N, P Co-Doped Carbon: In Situ Transition to (Oxy)hydroxide Phases During Oxygen Evolution Reaction
title Controlled Synthesis of Nickel Phosphides in Hollow N, P Co-Doped Carbon: In Situ Transition to (Oxy)hydroxide Phases During Oxygen Evolution Reaction
spellingShingle Controlled Synthesis of Nickel Phosphides in Hollow N, P Co-Doped Carbon: In Situ Transition to (Oxy)hydroxide Phases During Oxygen Evolution Reaction
Ríos Ruiz, D.
co-doped carbon
electrocatalyst
hollow nanostructures
nickel phosphide
oxygen evolution reaction
polydopamine
solvothermal method
title_short Controlled Synthesis of Nickel Phosphides in Hollow N, P Co-Doped Carbon: In Situ Transition to (Oxy)hydroxide Phases During Oxygen Evolution Reaction
title_full Controlled Synthesis of Nickel Phosphides in Hollow N, P Co-Doped Carbon: In Situ Transition to (Oxy)hydroxide Phases During Oxygen Evolution Reaction
title_fullStr Controlled Synthesis of Nickel Phosphides in Hollow N, P Co-Doped Carbon: In Situ Transition to (Oxy)hydroxide Phases During Oxygen Evolution Reaction
title_full_unstemmed Controlled Synthesis of Nickel Phosphides in Hollow N, P Co-Doped Carbon: In Situ Transition to (Oxy)hydroxide Phases During Oxygen Evolution Reaction
title_sort Controlled Synthesis of Nickel Phosphides in Hollow N, P Co-Doped Carbon: In Situ Transition to (Oxy)hydroxide Phases During Oxygen Evolution Reaction
dc.creator.none.fl_str_mv Ríos Ruiz, D.
Arévalo Cid, Pablo
Cebollada Borao, Jesús
Celorrio, V.
Haeussler, M.
Drev, S.
Martínez Huerta, M. Victoria
author Ríos Ruiz, D.
author_facet Ríos Ruiz, D.
Arévalo Cid, Pablo
Cebollada Borao, Jesús
Celorrio, V.
Haeussler, M.
Drev, S.
Martínez Huerta, M. Victoria
author_role author
author2 Arévalo Cid, Pablo
Cebollada Borao, Jesús
Celorrio, V.
Haeussler, M.
Drev, S.
Martínez Huerta, M. Victoria
author2_role author
author
author
author
author
author
dc.contributor.none.fl_str_mv Comunidad de Madrid
Agencia Estatal de Investigación (España)
Ministerio de Ciencia e Innovación (España)
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv co-doped carbon
electrocatalyst
hollow nanostructures
nickel phosphide
oxygen evolution reaction
polydopamine
solvothermal method
topic co-doped carbon
electrocatalyst
hollow nanostructures
nickel phosphide
oxygen evolution reaction
polydopamine
solvothermal method
description Developing sustainable and efficient electrocatalysts for the oxygen evolution reaction (OER) is crucial for advancing energy storage technologies. This study explored the dual role of phosphorus as a dopant in carbon matrices and a key component in nickel phosphides (Ni<inf>2</inf>P and Ni<inf>12</inf>P<inf>5</inf>), synthesized using dopamine (PDA) and ammonium phosphate as eco-friendly precursors. The phase formation of nickel phosphides was found to be highly dependent on the P/PDA ratio (0.15, 0.3, 0.6, and 0.9), allowing for the selective synthesis of Ni<inf>2</inf>P or Ni<inf>12</inf>P<inf>5</inf>. Operando Raman spectroscopy revealed that both phases undergo surface transformation into nickel (oxy)hydroxide species under OER conditions, yet Ni<inf>2</inf>P-based catalysts demonstrated superior activity and long-term stability. This enhancement is attributed to efficient electron transfer at the dynamic Ni<inf>2</inf>P/NiOOH interface. Additionally, hollow nanostructures formed at intermediate P/PDA ratios (≤0.3) via the Kirkendall effect and Ostwald ripening contributed to an increased specific surface area and micropore volume, further improving the catalytic performance. Electrochemical impedance spectroscopy confirmed reduced interfacial resistance and enhanced charge transport. These findings offer new insights into the rational design of high-performance electrocatalysts and propose a green, tunable synthesis approach for advanced energy conversion applications. © 2025 by the authors.
publishDate 2025
dc.date.none.fl_str_mv 2025
2026
2026
dc.type.none.fl_str_mv info:eu-repo/semantics/article
http://purl.org/coar/resource_type/c_6501
Publisher's version
info:eu-repo/semantics/publishedVersion
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/10261/419754
https://www.scopus.com/inward/record.uri?eid=2-s2.0-105001271300&doi=10.3390%2Fcatal15030292&partnerID=40&md5=11c89e4119373391cd68e2e968acc4a2
url http://hdl.handle.net/10261/419754
https://www.scopus.com/inward/record.uri?eid=2-s2.0-105001271300&doi=10.3390%2Fcatal15030292&partnerID=40&md5=11c89e4119373391cd68e2e968acc4a2
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv #PLACEHOLDER_PARENT_METADATA_VALUE#
info:eu-repo/grantAgreement///
Catalysts
https://doi.org/10.3390/catal15030292
Sí
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Multidisciplinary Digital Publishing Institute
publisher.none.fl_str_mv Multidisciplinary Digital Publishing Institute
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)
reponame_str DIGITAL.CSIC. Repositorio Institucional del CSIC
collection DIGITAL.CSIC. Repositorio Institucional del CSIC
repository.name.fl_str_mv
repository.mail.fl_str_mv
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score 15,811543

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