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We discuss the synthesis of a composite of ZrO 2 nanoparticles supported on multiwalled carbon nanotubes (MWCNT). Using X-ray diffraction and high-resolution transmission electron microscopy (HR-TEM), the ZrO 2 were found to be 2−3 nm tetragonal crystalline nanoparticles. Strong interfacial interaction between the ZrO 2 nanoparticles and the MWCNT surface was observed by near-edge X-ray absorption fine structure spectroscopy (NEXAFS) at the carbon K-edge and the oxygen K-edge, and this strong metal oxide/support interaction leads to small ZrO 2 particle size and thermal stability. The ZrO 2 /MWCNT was converted into a solid acid catalyst by sulfation, and the properties of S-ZrO 2 / MWCNT were studied. The nature of the acid sites was probed by S K-edge and Zr L-edges (L 3 , L 2 , L 1 ) XANES as well as catalytic probe reaction of cyclohexane dehydrogenation/cracking. Such composites would be good candidates for potential catalysis applications in fuel cell electrodes and biomass processing.

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