Abstract: | In situ monitoring of hydrogen peroxide (H2O2) during its production process is needed. Here, an electrochemical H2O2 sensor with a wide linear current response range (concentration: 5 × 10?8 to 5 × 10?2 m ), a low detection limit (32.4 × 10?9 m ), and a high sensitivity (568.47 µA mm ?1 cm?2) is developed. The electrocatalyst of the sensor consists of cobalt nanoparticles and atomic Co‐Nx moieties anchored on nitrogen doped carbon nanotube arrays (Co‐N/CNT), which is obtained through the pyrolysis of the sandwich‐like urea@ZIF‐67 complex. More cobalt nanoparticles and atomic Co‐Nx as active sites are exposed during pyrolysis, contributing to higher electrocatalytic activity. Moreover, a portable screen‐printed electrode sensor is constructed and demonstrated for rapidly detecting (cost ≈40 s) H2O2 produced in microbial fuel cells with only 50 µL solution. Both the synthesis strategy and sensor design can be applied to other energy and environmental fields. |