| Summary: | In this contribution, the three Mn-Zr catalysts with Mn<sub>x</sub>Zr<sub>1−x</sub>O<sub>2</sub> hybrid phase were synthesized by two-step precipitation route (TP), conventional coprecipitation method (CP) and ball milling process (MP). The components, textural and redox properties of the Mn-Zr hybrid catalysts were studied via XRD, BET, XPS, HR-TEM, H<sub>2</sub>-TPR. Regarding the variation of synthesis routes, the TP and CP routes offer a more obvious advantage in the adjustment of the concentration of Mn<sub>x</sub>Zr<sub>1−x</sub>O<sub>2</sub> solid solution compared to the MP process, which directly commands the content of Mn<sup>4+</sup> and oxygen vacancy and lattice oxygen, and thereby leads to the enhanced mobility of reactive oxygen species and catalytic activity for toluene combustion. Moreover, the TP-Mn2Zr3 catalyst with the enriched exposure content of 51.4% for the defective (111) lattice plane of Mn<sub>x</sub>Zr<sub>1−x</sub>O<sub>2</sub> exhibited higher catalytic activity and thermal stability for toluene oxidation than that of the CP-Mn2Zr3 sample with a value of 49.3%. This new observation will provide a new perspective on the design of bimetal catalysts with a higher VOCs combustion abatement.
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