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Recently, metal\u2010free heteroatom doped carbons are proposed as promising cost\u2010effective electrocatalysts for CO<jats:sub>2<\/jats:sub> reduction reaction (CO<jats:sub>2<\/jats:sub>RR). However, the lack of understanding of the active site prevents the realization of a high\u2010performance electrocatalyst for the CO<jats:sub>2<\/jats:sub>RR. Herein, we synthesized metal\u2010free N, P co\u2010doped carbons (NPCs) for producing syngas, which is composed of H<jats:sub>2<\/jats:sub> and CO, by CO<jats:sub>2<\/jats:sub> electrolysis using inexpensive bio\u2010based raw materials via simple pyrolysis. The syngas ratio (H<jats:sub>2<\/jats:sub>\/CO) can be controlled within the high demand range (0.3\u20134) at low potentials using NPCs by tuning the N and P contents. In comparison with only N doping or P doping, N and P co\u2010doping has a positive impact on improving CO<jats:sub>2<\/jats:sub>RR activity. Experimental analysis and density functional theory (DFT) calculations revealed that negatively charged C atoms adjacent to N and P atoms are the most favorable active sites for CO<jats:sub>2<\/jats:sub>\u2010to\u2010CO conversion compared to pyridinic N on N, P co\u2010doped carbon. Introducing N atoms generates the preferable CO<jats:sub>2<\/jats:sub> adsorption site, and P atoms contribute to decreasing the Gibbs free energy barrier for key *COOH intermediates adsorbed on the negatively charged C atoms.<\/jats:p>","DOI":"10.1002\/cssc.202402249","type":"journal-article","created":{"date-parts":[[2024,11,21]],"date-time":"2024-11-21T04:59:28Z","timestamp":1732165168000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["Metal\u2010Free N, P\u2010Codoped Carbon for Syngas Production with Tunable Composition via CO<sub>2<\/sub> Electrolysis: Addressing the Competition Between CO<sub>2<\/sub> Reduction and H<sub>2<\/sub> Evolution"],"prefix":"10.1002","volume":"18","author":[{"given":"Ryuji","family":"Takada","sequence":"first","affiliation":[{"name":"Division of Chemical Engineering Department of Materials Engineering Science Graduate School of Engineering Science Osaka University  1-3 Machikaneyama Toyonaka Osaka 560-8531 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hiroyuki","family":"Okada","sequence":"additional","affiliation":[{"name":"Center for Research on Green Sustainable Chemistry Tottori University  4-101 Koyama, Tottori Tottori 680-0945 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Kotaro","family":"Narimatsu","sequence":"additional","affiliation":[{"name":"Division of Chemical Engineering Department of Materials Engineering Science Graduate School of Engineering Science Osaka University  1-3 Machikaneyama Toyonaka Osaka 560-8531 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9868-5391","authenticated-orcid":false,"given":"Koji","family":"Miyake","sequence":"additional","affiliation":[{"name":"Division of Chemical Engineering Department of Materials Engineering Science Graduate School of Engineering Science Osaka University  1-3 Machikaneyama Toyonaka 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