α-FeO nanoparticles (NPs) with morphologies varying from shuttle to drum were synthesized through an anion-assisted and surfactant-free hydrothermal method by simply varying the ratios of ethanol and water in solvent. Control experiments show that the structural evolution can be attributed to a small-molecular-induced anisotropic growth mechanism in which the growth rate of α-FeO NPs along the a-, b-, or c-axis was well-controlled. The detailed structural analysis through the high-resolution transmission electron microscope (HRTEM) indicated that shuttle-like FeO NP surface was covered by high-density atomic steps, which endowed them with the enhanced adsorption and sensor ability toward dopamine (DA). The XPS characterizations indicated that the percentages of the O component follow the order of shuttle-like FeO (S-FeO for short) > pseudoshuttle-like FeO (Ps-FeO for short) > polyhedron-like FeO (Ph-FeO for short) > drum-like FeO (D-FeO for short). Benefits from these structural advantages, the S-FeO NPs-Nafion composite electrode exhibited remarkable electrochemical detection ability with a wide liner range from 0.2 μM to 0.107 mM and a low detection limit of 31.25 nM toward DA in the presence of interferents.

The oxygen reduction reaction (ORR) is of great importance in energy‐converting processes such as fuel cells and in metal–air batteries and is vital to facilitate the transition toward a nonfossil dependent society. The ORR has been associated with expensive noble metal catalysts that facilitate the O2 adsorption, dissociation, and subsequent electron transfer. Single‐ or few‐atom motifs based on earth‐abundant transition metals, such as Fe, Co, and Mo, combined with nonmetallic elements, such as P, S, and N, embedded in a carbon‐based matrix represent one of the most promising alternatives. Often these are referred to as single atom catalysts; however, the coordination number of the metal atom as well as the type and nearest neighbor configuration has a strong influence on the function of the active sites, and a more adequate term to describe them is metal‐coordinated motifs. Despite intense research, their function and catalytic mechanism still puzzle researchers. They are not molecular systems with discrete energy states; neither can they fully be described by theories that are adapted for heterogeneous bulk catalysts. Here, recent results on single‐ and few‐atom electrocatalyst motifs are reviewed with an emphasis on reports discussing the function and the mechanism of the active sites.

Inspired by a sequential hydrolysis-precipitation mechanism, morphology-controllable hierarchical cupric oxide (CuO) nanostructures are facilely fabricated by a green water/ethanol solution-phase transformation of Cu(x)(OH)(2x-2)(SO4) precursors in the absence of any organic capping agents and without annealing treatment in air. Antlerite Cu3(OH)4(SO4) precursors formed in a low volume ratio between water and ethanol can transform into a two-dimensional (2D) hierarchical nanoporous CuO ribbon assembly of free-standing nanoneedle building blocks and hierarchical nanoneedle-aggregated CuO flowers. Brochantite Cu4(OH)6(SO4) precursors formed in a high volume ratio between water and ethanol can transform into hierarchical nanoplate-aggregated CuO nanoribbons and nanoflowers. Such 2D hierarchical nanoporous CuO ribbons serving as a promising electrode material for nonenzymatic glucose detection show high sensitivity, a low detection limit, fast amperometric response and good selectivity. Significantly, this green water-induced precursor-hydrolysis method might be used to control effectively the growth of other metal oxide micro-/nanostructures.

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