Abstract

The formation of a PdZn alloy from a 4.3% Pd/ZnO catalyst was characterized by combined in situ high-resolution X-ray diffraction (HRXRD) and X-ray absorption spectroscopy (XAS). Alloy formation started already at around 100 °C, likely at the surface, and reached the bulk with increasing temperature. The structure of the catalyst was close to the bulk value of a 1:1 PdZn alloy with a L1o structure (RPd−Pd = 2.9 A, RPd−Zn = 2.6 A, CNPd−Zn = 8, CNPd−Pd = 4) after reduction at 300 °C and above. The activity of the gas-phase hydrogenation of 1-pentyne decreased with the formation of the PdZn alloy. In contrast to Pd/SiO2, no full hydrogenation occurred over Pd/ZnO. Over time, only slight decomposition of the alloy occurred under reaction conditions.

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