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Photocatalytic non-oxidative coupling of methane (PNOCM) is a mild and cost-effective method for the production of multicarbon compounds. However, the separation of photogenerated charges and activation of methane (CH 4 ) are the main challenges for this reaction. Here, single crystal-like TiO 2 nanotubes (V O -p-TNTs) with oxygen vacancies (V O ) and preferential orientation were prepared and applied to PNOCM. The results demonstrate that the significantly enhanced photocatalytic performance is mainly related to the strong synergistic effect between preferential orientation and V O . The preferential orientation of V O -p-TNT along the [001] direction reduces the formation of complex centers at grain boundaries as the form of interfacial states and potential barriers, which improves the separation and transport of photogenerated carriers. Meanwhile, V O provides abundant coordination unsaturated sites for CH 4 chemisorption and also acts as electron traps to hinder the recombination of electrons and holes, establishing an effective electron transfer channel between the adsorbed CH 4 molecule and photocatalyst, thus weakening the C-H bond. In addition, the introduction of V O broadens the light absorption range. As a result, V O -p-TNT exhibits excellent PNOCM performance and provides new insights into catalyst design for CH 4 conversion.

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