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The electrocatalytic reduction of carbon dioxide into organic fuels and feedstocks is a fascinating method to implement the sustainable carbon cycle. Thus, a rational design of advanced electrocatalysts and a deep understanding of reaction mechanisms are crucial for the complex reactions of carbon dioxide reduction with multiple electron transfer. In situ and operando techniques with real‐time monitoring are important to obtain deep insight into the electrocatalytic reaction to reveal the dynamic evolution of electrocatalysts' structure and composition under experimental conditions. In this paper, the reaction pathways for the CO2 reduction reaction (CO2RR) in the generation of various products (e.g., C1 and C2) via the proposed mechanisms are introduced. Moreover, recent advances in the development and applications of in situ and operando characterization techniques, from the basic working principles and in situ cell structure to detailed applications are discussed. Suggestions and future directions of in situ/operando analysis are also addressed. [ABSTRACT FROM AUTHOR]

A series of CuCe0.75Zr0.25Ox catalysts (CCZ) were synthesized based on the environmental‐friendly bacterial cellulose (BC) by using the sol‐gel method. The corresponding synthesis mechanism, physicochemical properties of the catalysts and catalytic performances for toluene oxidation were comprehensively studied. In the presence of BC without sugar, the CCZ−A synthesized by ethanol‐gel exhibits better catalytic activity than the CCZ−W synthesized by water‐gel, which may be due to the different roles of BC in different solvents. However, it is worth noting that the graft copolymerization between BC and active metal (Ce4+, Cu2+) is the same process in both water‐gel and ethanol‐gel. The activity of CCZ‐SW synthesized by water‐gel using BC with sugar is obviously higher than that of CCZ−W and CCZ−A. The temperature of complete degradation of toluene over CCZ‐SW is 205 °C, which is 35 °C lower than that of CCZ−W. The results from BET, Raman and H2‐TPR indicate that the larger the specific surface area, the more oxygen vacancies and better low‐temperature reducibility, that are mainly responsible for the excellent activity of CCZ‐SW. The existence of sugar in BC could hinder the agglomeration of active metal particles during the calcination process. Combined with the results of in situ DRIFT, the adsorbed toluene on the catalyst surface is oxidized into alkoxide, aldehydic and carboxylic acid species as intermediates before the complete oxidation into CO2 and H2O. [ABSTRACT FROM AUTHOR]