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Electrochemical reduction of CO2 (CO2RR) into valuable hydrocarbons is appealing in alleviating the excessive CO2 level. We present the very first utilization of metallic bismuth–tin (Bi‐Sn) aerogel for CO2RR with selective HCOOH production. A non‐precious bimetallic aerogel of Bi‐Sn is readily prepared at ambient temperature, which exhibits 3D morphology with interconnected channels, abundant interfaces and a hydrophilic surface. Superior to Bi and Sn, the Bi‐Sn aerogel exposes more active sites and it has favorable mass transfer properties, which endow it with a high FEHCOOH of 93.9 %. Moreover, the Bi‐Sn aerogel achieves a FEHCOOH of ca. 90 % that was maintained for 10 h in a flow battery. In situ ATR‐FTIR measurements confirmed that the formation of *HCOO is the rate‐determining step toward formic acid generation. DFT demonstrated the coexistence of Bi and Sn optimized the energy barrier for the production of HCOOH, thereby improving the catalytic activity.

A variety of boehmite hollow core/shell and hollow microspheres with high adsorption affinity toward organic pollutants in water were prepared via a facile one-pot hydrothermal method using aluminum sulfate as a precursor and urea and sodium tartrate as precipitating and mediating agents, respectively. These microspheres were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and nitrogen adsorption. In addition, the aforementioned microspheres were examined as potential adsorbents for Congo red and phenol from aqueous solutions. This study shows that the crystallinity, specific surface area, and pore structure of the resulting microspheres can be controlled by varying the concentration of sodium tartrate and reaction time. The reported experiments allowed us to propose the mechanism of formation of hollow core/shell and hollow microspheres, which involves sodium tartrate-mediated phase transformation, followed by a subsequent self-assembly process. Adsorption performance of the boehmite microspheres studied is gradually enhanced with increasing concentration of sodium tartrate. This enhancement is substantial in comparison to the performance of the microspheres prepared without sodium tartrate and commercial boehmite powders, and it is probably due to several factors, such as high specific surface area, large pore volume, proper crystallite size, and unique core/shell morphology and structure of the aforementioned microspheres. Especially, the hollow core/shell microspheres prepared at 0.01 M concentration of sodium tartrate exhibited the best adsorption performance, which can be easily regenerated without any great loss in the adsorption capacity. This study suggests that the degree of chemical self-transformation of amorphous particles into crystalline shells, followed by their self-assembly into complex higher-order architectures with desirable functionality, can be mediated by simple organic anions.

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