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Orderly heterostructured catalysts, which integrate nanomaterials of complementary structures and dimensions into single‐entity structures, have hold great promise for sustainability applications. In this work, it is showcased that air as green reagent can trigger in situ localized phase transformation and transform the metal carbonate hydroxide nanowires into ordered heterostructured catalyst. In single‐crystal nanowire heterostructure, the in situ generated and nanosized Co3O4 will be anchored in single‐crystal Co6(CO3)2(OH)8 nanowires spontaneously, triggered by the lattice matching between the (220) plane of Co3O4 and the (001) plane of Co6(CO3)2(OH)8. The lattice matching allows intimate contact at heterointerface with well‐defined orientation and strong interfacial coupling, and thus significantly expedites the transfer of photogenerated electrons from tiny Co3O4 to catalytically active Co6(CO3)2(OH)8 in single‐crystal nanowire, which elevates the catalytic efficiency of metal carbonate catalyst in the CO2 reduction reaction (VCO = 19.46 mmol g−1 h−1 and VH2 = 11.53 mmol g−1 h−1). The present findings add to the growing body of knowledge on exploiting Earth‐abundant metal‐carbonate catalysts, and demonstrate the utility of localized phase transformation in constructing advanced catalysts for energy and environmental sustainability applications.

The heterojunction effect can effectively improve the separation efficiency of the photocatalyst's photo-generated electron and hole pairs, thereby greatly improving the photocatalytic hydrogen production performance of the photocatalyst. In this paper, Bi 6 O 6 (OH) 3 (NO 3 ) 3 • 1.5H 2 O (BBN) and ZnO are used to construct and synthesize Bi 6 O 6 (OH) 3 (NO 3 ) 3 • 1.5H 2 O/ZnO (BBN/ZnO) heterojunction photocatalyst. Under UV-vis light irradiation, the BBN/ZnO composite could generate H 2 with a rate of 28.66 μmol•g −1 •h −1 , which is higher than pure BBN (0.92 μmol•g −1 •h −1 ) and ZnO (6.54 μmol•h −1 •g −1 ) at around 31.1 and 4.4 times, respectively. Moreover, the experimental results found that the composite still exhibits excellent photocatalytic activity and maintains a high and stable activity in the 12-hour experiment with 3 cycles. The possible mechanism to enhance the photocatalytic behavior is attributed to the expanded light absorption range, reduced surface migration resistance, and inhibited recombination of photo-generated electron and hole pairs.