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Herein, an in situ assembly strategy is developed for preparing the P, N co\u2010doped carbon nanotubes and Mo\/MoS<jats:sub>2(1\u2212<\/jats:sub><jats:italic><jats:sub>x<\/jats:sub><\/jats:italic><jats:sub>\u2212<\/jats:sub><jats:italic><jats:sub>y<\/jats:sub><\/jats:italic><jats:sub>)<\/jats:sub>P<jats:italic><jats:sub>x<\/jats:sub><\/jats:italic> nanosheets composites (Mo\/MoS<jats:sub>2(1\u2212<\/jats:sub><jats:italic><jats:sub>x<\/jats:sub><\/jats:italic><jats:sub>\u2212<\/jats:sub><jats:italic><jats:sub>y<\/jats:sub><\/jats:italic><jats:sub>)<\/jats:sub>P<jats:italic><jats:sub>x<\/jats:sub><\/jats:italic>@PNC) for hydrogen evolution reactions (HER). The PNC guarantees structural stability and fast charge transfer in a long\u2010range, while Mo\/MoS<jats:sub>2(1\u2212<\/jats:sub><jats:italic><jats:sub>x<\/jats:sub><\/jats:italic><jats:sub>\u2212<\/jats:sub><jats:italic><jats:sub>y<\/jats:sub><\/jats:italic><jats:sub>)<\/jats:sub>P<jats:italic><jats:sub>x<\/jats:sub><\/jats:italic> nanosheets offer a large electrochemically active surface area with embedded metallic Mo in improving its internal conductivity and rich surface\/interface properties. Thus, the optimized catalyst (Mo\/MoS<jats:sub>1.15<\/jats:sub>P<jats:sub>0.30<\/jats:sub>@PNC) possesses more surface active sites and exhibits extraordinary HER activities, with a small overpotential of \u221279 and \u2212131\u00a0mV at 10\u00a0mA cm<jats:sup>\u22121<\/jats:sup>, and low Tafel slope of 49 and 82\u00a0mV dec<jats:sup>\u22121<\/jats:sup> in 0.5 <jats:sc>m<\/jats:sc> H<jats:sub>2<\/jats:sub>SO<jats:sub>4<\/jats:sub> and 1.0 <jats:sc>m<\/jats:sc> KOH, respectively. Density functional theory calculations confirm that the higher substitution of S atoms by P in MoS<jats:sub>2<\/jats:sub> can form strong Mo 3d\u2010S 2p\u2010P 2p hybridizations at Fermi level, resulting in the narrower bandgap and smaller \u2206<jats:italic>G<\/jats:italic><jats:sub>H<\/jats:sub><jats:italic><jats:sub>*<\/jats:sub><\/jats:italic> of hydrogen (H*) adsorption, thereby leading to the promoted HER activity.<\/jats:p>","DOI":"10.1002\/smll.202004973","type":"journal-article","created":{"date-parts":[[2020,11,26]],"date-time":"2020-11-26T09:46:37Z","timestamp":1606383997000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":41,"title":["Hierarchical Ultrathin Mo\/MoS<sub>2(1\u2212<\/sub><i><sub>x<\/sub><\/i><sub>\u2212<\/sub><i><sub>y<\/sub><\/i><sub>)<\/sub>P<i><sub>x<\/sub><\/i> Nanosheets Assembled on P, N Co\u2010Doped Carbon Nanotubes for Hydrogen Evolution in Both Acidic and Alkaline Electrolytes"],"prefix":"10.1002","volume":"16","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-7710-7912","authenticated-orcid":false,"given":"Xiaojun","family":"Zhao","sequence":"first","affiliation":[{"name":"Key Laboratory for Macromolecular Science of Shaanxi Province School of Chemistry and Chemical Engineering Shaanxi Normal University  Xi'an 710062 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yibing","family":"Li","sequence":"additional","affiliation":[{"name":"School of Chemistry University of New South Wales  Sydney New South Wales 2052 Australia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chuan","family":"Zhao","sequence":"additional","affiliation":[{"name":"School of Chemistry University of New South Wales  Sydney New South Wales 2052 Australia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5082-5180","authenticated-orcid":false,"given":"Zhi\u2010Hong","family":"Liu","sequence":"additional","affiliation":[{"name":"Key Laboratory for Macromolecular Science of Shaanxi Province School of Chemistry and Chemical Engineering Shaanxi Normal University  Xi'an 710062 P. R. 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