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However, synthesis of high\u2010purity unconventional\u2010phase noble metal nanomaterials remains highly challenging via current wet\u2010chemical methods. Herein, we develop a unique synthetic methodology to prepare freestanding unconventional hexagonal close\u2010packed (2H) Rh nanoplates (NPLs) via a rationally designed two\u2010step strategy. By extracting C from pre\u2010synthesized rhodium carbide of different sizes and morphology, phase\u2010controlled synthesis of Rh nanomaterials can be achieved. Impressively, the obtained parallelogram 2H Rh NPLs have high phase purity, well\u2010defined 2H (0001)\n                    <jats:sub>h<\/jats:sub>\n                    and (100)\n                    <jats:sub>h<\/jats:sub>\n                    facets, and good thermostability (stable up to 300\u00a0\u00b0C). In the proof\u2010of\u2010concept electrocatalytic nitrate reduction reaction (NO\n                    <jats:sub>3<\/jats:sub>\n                    RR), the 2H Rh NPLs achieve higher ammonia (NH\n                    <jats:sub>3<\/jats:sub>\n                    ) Faradaic efficiency (91.9%) and NH\n                    <jats:sub>3<\/jats:sub>\n                    yield rate (156.97\u00a0mg h\n                    <jats:sup>\u22121<\/jats:sup>\n                    mg\n                    <jats:sub>cat<\/jats:sub>\n                    <jats:sup>\u22121<\/jats:sup>\n                    ) with lower overpotentials compared to the conventional face\u2010centered cubic (3C) Rh nanocubes with (100)\n                    <jats:sub>f<\/jats:sub>\n                    facets. Density functional theory calculations reveal that the unconventional (0001)\n                    <jats:sub>h<\/jats:sub>\n                    surface has energetically favored NO\n                    <jats:sub>3<\/jats:sub>\n                    RR pathway and stronger H\n                    <jats:sup>*<\/jats:sup>\n                    absorption ability compared to the (100)\n                    <jats:sub>f<\/jats:sub>\n                    surface, which may lead to the higher activity and selectivity of NH\n                    <jats:sub>3<\/jats:sub>\n                    production on 2H Rh NPLs. This work opens new avenues to the rational synthesis of unconventional\u2010phase metal nanomaterials and provides important guidelines to design high\u2010performance electrocatalysts.\n                  <\/jats:p>","DOI":"10.1002\/anie.202500985","type":"journal-article","created":{"date-parts":[[2025,3,28]],"date-time":"2025-03-28T10:07:27Z","timestamp":1743156447000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":28,"title":["Carbon\u2010Extraction\u2010Triggered Phase Engineering of Rhodium Nanomaterials for Efficient Electrocatalytic Nitrate Reduction Reaction"],"prefix":"10.1002","volume":"64","author":[{"given":"Long","family":"Zheng","sequence":"first","affiliation":[{"name":"Department of Chemistry The Chinese University of Hong Kong  Hong Kong China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yan","family":"Zhang","sequence":"additional","affiliation":[{"name":"Department of Chemical and Biological Engineering The Hong Kong University of Science and Technology  Clear Water Bay Kowloon Hong Kong China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Weiwei","family":"Chen","sequence":"additional","affiliation":[{"name":"Beijing National Laboratory for Condensed Matter Physics Institute of Physics Chinese Academy of Sciences  Beijing 100190 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiangou","family":"Xu","sequence":"additional","affiliation":[{"name":"Key Laboratory of Quantum Materials and Devices of Ministry of Education School of Physics Southeast University  Nanjing 211189 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ruiqi","family":"Zhang","sequence":"additional","affiliation":[{"name":"Beijing National Laboratory for Molecular Sciences New Cornerstone Science Laboratory College of Chemistry and Molecular Engineering Peking University  Beijing 100871 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University of Hong Kong  Hong Kong China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gang","family":"Wang","sequence":"additional","affiliation":[{"name":"Department of Chemistry The Chinese University of Hong Kong  Hong Kong China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chen","family":"Ma","sequence":"additional","affiliation":[{"name":"Department of Chemistry The Chinese University of Hong Kong  Hong Kong China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Lei","family":"Xu","sequence":"additional","affiliation":[{"name":"Department of Chemistry The Chinese University of Hong Kong  Hong Kong China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Peng","family":"Han","sequence":"additional","affiliation":[{"name":"Department of Chemistry The Chinese University of Hong Kong  Hong Kong 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Ministry of Education School of Physics Southeast University  Nanjing 211189 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Dong","family":"Su","sequence":"additional","affiliation":[{"name":"Beijing National Laboratory for Condensed Matter Physics Institute of Physics Chinese Academy of Sciences  Beijing 100190 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Minhua","family":"Shao","sequence":"additional","affiliation":[{"name":"Department of Chemical and Biological Engineering The Hong Kong University of Science and Technology  Clear Water Bay Kowloon Hong Kong China"},{"name":"Guangzhou Key Laboratory of Electrochemical Energy Storage Technologies, Fok Ying Tung Research Institute The Hong Kong University of Science and Technology  Guangzhou 511458 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ye","family":"Chen","sequence":"additional","affiliation":[{"name":"Department of Chemistry The Chinese University of 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