XRD and XPS Study of Cu−Ni Interactions on Reduced Copper−Nickel−Aluminum Oxide Solid Solution Catalysts

Copper−nickel−aluminum oxide solid solutions were reduced in hydrogen to produce alumina-supported copper−nickel alloy catalysts. XRD patterns of reduced oxides showed that the type of active metals which emerged upon reduction were sensitive to the reduction temperature and the copper content. Variations from +0.8 to +1 eV were found in the experimental Ni 2p3/2 binding energy (BE) of nickel in the solid solutions compared to the experimental Ni 2p3/2 BE of bulk nickel, attributed to the Ni−Ni arrangements in the solid solution. Also, when the curve-fitted BE values of Ni 2p3/2 and Cu 2p3/2 of different reduced solid solutions were compared, it was found that copper and nickel were in different chemical states depending on reduction temperature and the amount of the copper. Changes in Ni 2p3/2 BE in the reduced solid solutions were also discussed in terms of the filling of nickel d-hole bands due to nickel−copper d−d band interactions. At both high copper content and reduction temperature, copper had a tendency to segregate in order to reduce the interfacial surface energies. This was postulated based on the observation that the Ni 2p3/2 curve-fitted BE values were restored to somewhat close to bulk nickel at a copper content of 11 mol % and reduction temperature of 700 °C.