| Summary: | This study reports a novel Ni(OH)<sub>2</sub>/Co<sub>3</sub>O<sub>4</sub> heterostructured nanomaterial synthesized through a simple two-step hydrothermal method combined with subsequent heat treatment. The Ni(OH)<sub>2</sub>/Co<sub>3</sub>O<sub>4</sub> heterostructured nanomaterial showed excellent performance in the detection of xylene gas. XRD, SEM, and EDS characterized the crystal structure, microstructure, and composition elements of Co<sub>3</sub>O<sub>4</sub> and Ni(OH)<sub>2</sub>/Co<sub>3</sub>O<sub>4</sub>, and the gas sensing properties of the Co<sub>3</sub>O<sub>4</sub> sensor and Ni(OH)<sub>2</sub>/Co<sub>3</sub>O<sub>4</sub> sensor were systematically tested. The test results indicate the Ni(OH)<sub>2</sub>/Co<sub>3</sub>O<sub>4</sub> sensor has an optimal operating temperature of 175 °C, which is 10 °C lower than that of the Co<sub>3</sub>O<sub>4</sub> sensor; has a response of 14.1 to 100 ppm xylene, which is 7-fold higher than that of the Co<sub>3</sub>O<sub>4</sub> sensor; reduces the detection limit of xylene from 2 ppm to 100 ppb; and has at least a 4-fold higher response to xylene than other gases. The Ni(OH)<sub>2</sub>/Co<sub>3</sub>O<sub>4</sub> nanocomposite exerts the excellent catalytic performance of two-dimensional nanomaterial Ni(OH)<sub>2</sub>, solves the deficiency in the electrical conductivity of Ni(OH)<sub>2</sub> materials, and realizes the outstanding sensing performance of xylene, while the construction of the p–n heterojunction between Ni(OH)<sub>2</sub> and Co<sub>3</sub>O<sub>4</sub> also improves the sensing performance of the material. This study provides a strategy for designing high-performance xylene gas sensors using two-dimensional Ni(OH)<sub>2</sub> materials.
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