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Although being attractive materials for photoelectrochemical hydrogen evolution reaction (PEC HER) under neutral or acidic conditions, conjugated polymers still show poor PEC HER performance in alkaline medium due to the lack of water dissociation sites. Herein, we demonstrate that tailoring the polymer skeleton from poly(diethynylthieno[3,2‐b]thiophene) ( pDET ) to poly(2,6‐diethynylbenzo[1,2‐b:4,5‐b′]dithiophene ( pBDT ) and poly(diethynyldithieno[3,2‐b:2′,3′‐d]thiophene) ( pDTT ) in conjugated acetylenic polymers (CAPs) introduces highly efficient active sites for water dissociation. As a result,  pDTT  and  pBDT , grown on Cu substrate, demonstrate benchmark photocurrent densities of 170 μA cm −2  and 120 μA cm −2  (at 0.3 V vs. RHE; pH 13), which are 4.2 and 3 times higher than that of  pDET , respectively. Moreover, by combining DFT calculations and electrochemical operando resonance Raman spectroscopy, we propose that the electron‐enriched C β  of the outer thiophene rings of  pDTT  are the water dissociation active sites, while the −C≡C− bonds function as the active sites for hydrogen evolution.

angewandte chemie international edition

Thiophene‐Based Conjugated Acetylenic Polymers with Dual Active Sites for Efficient Co‐Catalyst‐Free Photoelectrochemical Water Reduction in Alkaline Medium