2D–2D lattice engineering route is used to synthesize intimately coupled nanohybrids of layered double hydroxide (LDH) and potassium hexaniobate. The 2D–2D lattice engineering route is based on the electrostatically derived self-assembly of delaminated zinc-chromium-layered double hydroxide (ZC-LDH) nanosheets and potassium hexaniobate (HNb) nanosheets (ZCNb nanohybrids). The 2D–2D lattice-engineered ZCNb nanohybrids display expanded surface area, mesoporous anchored nanosheets network morphology, and intimate coupling between nanosheets. The 2D–2D lattice engineered ZCNb nanohybrids are used for the low temperature operated gas sensor. The ZCNb nanohybrids display outstanding selectivity for the SO2, with the high response of 61.5% compared to pristine ZC-LDH (28.08%) and potassium niobate (8%) at 150 °C. Moreover, ZCNb sensors demonstrate superior response and recovery periods of 6 and 167 s at 150 °C, respectively. This result underscores the exceptional functionality of the ZCNb nanohybrids as efficient SO2 sensors. Moreover, these findings vividly demonstrate that the 2D–2D lattice-engineered ZCNb nanohybrids are quite effective not only in improving the gas sensor activity but also in developing of new type of intimately coupled mesoporous LDH-metal-oxide based hybrid materials.

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