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This study reports Cu\/Co\u2010based core\u2010shell nanocrystals (NCs) showing excellent performance for both MOR and EOR. The structure, composition and size of the NCs can be controlled by adjusting the synthesis parameters in a one\u2010pot microwave\u2010assisted process. The electrocatalytic performance of the NCs shows lower potentials for both MOR and EOR compared to the OER. They consist of a copper\u2010rich metallic core initially encapsulated by a shell composed of cobalt oxide and cobalt carbide. This nanoheterostructure evolves to a copper oxide core surrounded by an oxide shell consisting of small cobalt\u2010 and copper\u2010oxide nanodomains upon chronopotentiometry experiments. The excellent performance in both MOR and EOR is attributed to the oxidation of the NCs and a concomitant diffusion process that forms small oxide clusters. The final structure provided NCs with high mass activities for both alcohol oxidation reactions, producing formic and acetic acid as products (for MOR and EOR, respectively). Finally, the NCs are tested for hybrid water electrolysis, demonstrating high hydrogen production along with high stability.<\/jats:p>","DOI":"10.1002\/advs.202505581","type":"journal-article","created":{"date-parts":[[2025,7,25]],"date-time":"2025-07-25T21:09:42Z","timestamp":1753477782000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["Microwave\u2010Assisted Synthesis of Cu\/Co\u2010Based Nanoheterostructures for High\u2010Efficiency Alcohol Oxidation"],"prefix":"10.1002","volume":"12","author":[{"given":"Xuesong","family":"Zhang","sequence":"first","affiliation":[{"name":"Institut de Ci\u00e8ncia de Materials de Barcelona (ICMAB\u2010CSIC) Campus Universitari  Bellaterra 08193 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jaume","family":"G\u00e1zquez","sequence":"additional","affiliation":[{"name":"Institut de Ci\u00e8ncia de Materials de Barcelona (ICMAB\u2010CSIC) Campus Universitari  Bellaterra 08193 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0160-2770","authenticated-orcid":false,"given":"Arturo","family":"Pajares","sequence":"additional","affiliation":[{"name":"Materials &amp; Chemistry Flemish Institute for Technological Research (VITO NV)  Boeretang 200 Mol 2400 Belgium"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0240-1011","authenticated-orcid":false,"given":"Dino","family":"Tonti","sequence":"additional","affiliation":[{"name":"Institut de Ci\u00e8ncia de Materials de Barcelona (ICMAB\u2010CSIC) Campus Universitari  Bellaterra 08193 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9076-4642","authenticated-orcid":false,"given":"Pablo","family":"Guardia","sequence":"additional","affiliation":[{"name":"Institut de Ci\u00e8ncia de Materials de Barcelona (ICMAB\u2010CSIC) Campus Universitari  Bellaterra 08193 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,7,25]]},"reference":[{"key":"e_1_2_9_1_1","doi-asserted-by":"publisher","DOI":"10.1038\/s43586-022-00164-0"},{"key":"e_1_2_9_2_1","doi-asserted-by":"publisher","DOI":"10.1007\/s10311-021-01322-8"},{"key":"e_1_2_9_3_1","doi-asserted-by":"publisher","DOI":"10.1021\/acscatal.8b02712"},{"key":"e_1_2_9_4_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.nanoen.2017.05.022"},{"key":"e_1_2_9_5_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.accounts.8b00002"},{"key":"e_1_2_9_6_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202214333"},{"key":"e_1_2_9_7_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.gce.2022.11.001"},{"key":"e_1_2_9_8_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202213328"},{"key":"e_1_2_9_9_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.mser.2024.100829"},{"key":"e_1_2_9_10_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41570-019-0084-4"},{"key":"e_1_2_9_11_1","doi-asserted-by":"publisher","DOI":"10.1039\/D1MA00503K"},{"key":"e_1_2_9_12_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.202211099"},{"key":"e_1_2_9_13_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.ijhydene.2021.06.027"},{"key":"e_1_2_9_14_1","doi-asserted-by":"publisher","DOI":"10.1002\/smll.202006623"},{"key":"e_1_2_9_15_1","doi-asserted-by":"publisher","DOI":"10.1039\/D2EE03936B"},{"key":"e_1_2_9_16_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.cej.2022.139797"},{"key":"e_1_2_9_17_1","doi-asserted-by":"publisher","DOI":"10.1002\/adfm.202106401"},{"key":"e_1_2_9_18_1","doi-asserted-by":"publisher","DOI":"10.1039\/C4EE03746D"},{"key":"e_1_2_9_19_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jechem.2024.06.045"},{"key":"e_1_2_9_20_1","doi-asserted-by":"publisher","DOI":"10.1002\/advs.202309813"},{"key":"e_1_2_9_21_1","doi-asserted-by":"publisher","DOI":"10.1039\/D4GC00227J"},{"key":"e_1_2_9_22_1","doi-asserted-by":"publisher","DOI":"10.1039\/D2TA01104B"},{"key":"e_1_2_9_23_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.201502696"},{"key":"e_1_2_9_24_1","doi-asserted-by":"publisher","DOI":"10.1039\/C6RA27073E"},{"key":"e_1_2_9_25_1","doi-asserted-by":"publisher","DOI":"10.1002\/aenm.202103144"},{"key":"e_1_2_9_26_1","doi-asserted-by":"publisher","DOI":"10.1021\/acscatal.6b03021"},{"key":"e_1_2_9_27_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.apcatb.2018.12.017"},{"key":"e_1_2_9_28_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jelechem.2023.117532"},{"key":"e_1_2_9_29_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jtice.2021.06.054"},{"key":"e_1_2_9_30_1","volume":"15","author":"Saxena A.","year":"2023","journal-title":"ACS Appl. 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