Synthesis of Fully Exposed Single‐Atom‐Layer Metal Clusters on 2D Ordered Mesoporous TiO2 Nanosheets

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A sulfhydryl monomicelles interfacial assembly strategy is presented for the synthesis of fully exposed single‐atom‐layer Pt clusters on 2D mesoporous TiO2 (SAL‐Pt@mTiO2) nanosheets. This synthesis features the introduction of the sulfhydryl group in monomicelles to finely realize the controllable co‐assembly process of Pt precursors within ordered mesostructures. The resultant SAL‐Pt@mTiO2 shows uniform SAL Pt clusters (≈1.2 nm) anchored in ultrathin 2D nanosheets (≈7 nm) with a high surface area (139 m2 g−1), a large pore size (≈25 nm) and a high dispersion (≈99 %). Moreover, this strategy is universal for the synthesis of other SAL metal clusters (Pd and Au) on 2D mTiO2 with high exposure and accessibility. When used as a catalyst for hydrogenation of 4‐nitrostyrene, the SAL‐Pt@mTiO2 shows a high catalytic activity (TOF up to 2424 h−1), 100 % selectivity for 4‐aminostyrene, good stability, and anti‐resistance to thiourea poisoning under relatively mild conditions (25 °C, 10 bar).