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The fabrication of well‐defined, atomically sharp substrate surfaces over a wide range of lattice parameters is reported, which is crucial for atomically regulated epitaxial growth of complex oxide heterostructures. By applying a framework for controlled selective wet etching of complex oxides on the stable rare‐earth scandates (REScO3), apseudocubic = 0.394 – 0.404 nm, the large chemical sensitivity of REScO3 to basic solutions is exploited, which results in reproducible, single‐terminated surfaces. Time‐of‐flight mass‐spectroscopy measurements show that after wet etching the surfaces are predominantly ScO2 ‐terminated. Moreover, the morphology study of SrRuO3 thin‐film growth gives no evidence for mixed termination. Therefore, it is concluded that the REScO3 surfaces are completely ScO2 ‐terminated.

Two-dimensional (2D) (hydro)oxide materials, that is, nanosheets, enable the preparation of advanced 2D materials and devices. The general synthesis route of nanosheets involves exfoliating layered metal (hydro)oxide crystals. This exfoliation process is considered to be time-consuming, hindering their industrial-scale production. Based on in situ exfoliation studies on the protonated layered titanate H(1.07)Ti(1.73)O4⋅H2O (HTO), it is now shown that ion intercalation-assisted exfoliation driven by chemical reaction provides a viable and fast route to isolated nanosheets. Contrary to the general expectation, data indicate that direct exfoliation of HTO occurs within seconds after mixing of the reactants, instead of proceeding via a swollen state as previously thought. These findings reveal that ion intercalation-assisted exfoliation driven by chemical reaction is a promising exfoliation route for large-scale synthesis.

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The nature of the external crystal facets is critical to control the (photo)catalytic properties. Two-dimensional materials can expose only one type of crystal facet among zero-dimensional (0D), one-dimensional (1D), and two-dimensional (2D) materials. Controllable tuning of the nature of the external crystal facets of 2D materials is highly desirable but very challenging. Here, we show that 2D particles with the desirable crystal facet for high-performance photocatalytic H2 generation can be obtained by using 2D metal oxide materials (i.e., nanosheets of Ca2Nb3O10 and Ti0.87O2) as templates taking consideration of the crystal configuration of 2D oxide and target compounds. We demonstrate that anatase TiO2 crystals grown on different nanosheet templates exhibit variations in photocatalytic hydrogen production rates from aqueous phase methanol solutions (6.7%), which can be attributed to the nature of the main crystal facet exposed. In view of the large number of 2D materials that have already been synthesized, this work offers a key to design and synthesize nanoparticles with the desirable specific external crystal facet for (photo)catalysis application.