A novel Ni@hollow silicate zirconia (Ni@HSZ) is prepared via a hydrothermal approach to re-use the SiO₂ in Ni@SiO₂@ZrO₂ with TBAOH as an etchant and template. The catalyst was characterized using a combination of XRD, TEM, ICP-OES, N₂-isotherms, H₂-TPR, H₂-TPD, XPS, TGA, and Raman techniques. The catalyst is evaluated time-on-stream and its high catalytic activity and coking resistance capability are identified. From the characterization of XRD, TEM, Raman, XPS, and TGA, the Ni@HSZ has the capability of resisting carbon deposition during dry reforming of methane for 50 hours while maintaining high catalytic performance.