AVS 65th International Symposium & Exhibition
    Processing and Characterization of Air-Liquid, Solid-Liquid and Air-Solid Interfaces Focus Topic Tuesday Sessions
       Session PC+AS+BI+EM+NS+PB+SS-TuA

Paper PC+AS+BI+EM+NS+PB+SS-TuA11
Atomic Scale Observation of Oxidation and Reduction of Palladium Surface

Tuesday, October 23, 2018, 5:40 pm, Room 202A

Session: Progress in Industrial Processes and Characterization of Interfaces and Gas-Solid Interfacial Processes and Characterization
Presenter: Takehiro Tamaoka, Osaka University, Japan
Authors: T. Tamaoka, Osaka University, Japan
H. Yoshida, Osaka University, Japan
S. Takeda, Osaka University, Japan
Correspondent: Click to Email

Reaction processes on metal surfaces under gas environment have been investigated in various research fields such as catalysis, gas sensing, and many more. Palladium is a well–known material which is used for hydrogen storage, hydrogen sensing, and exhaust catalysis. Therefore, the phase transition of palladium in hydrogen or oxygen has been extensively investigated by means of environmental transmission electron microscopy (ETEM). However, the oxidation and reduction process of palladium surface at the atomic scale remain poorly understood.

Here, we investigated the surface structure of a wedge–shaped palladium specimen in both hydrogen and oxygen by means of in-situ atomic resolution ETEM. Under ambient condition the surface of palladium is oxidized by several nanometers. After introducing hydrogen (100 Pa) in ETEM, the native oxide layer (PdO) was reduced to metallic fcc palladium even at room temperature. After exposure and exhaustion of hydrogen, we introduced oxygen (100 Pa) in ETEM. The palladium oxide was reproduced and the ETEM results show that the oxidation started from step edges and terraces and proceeded until the palladium surface was completely covered by the palladium oxide.

We also show that oxidation of palladium is dependent on the history of hydrogen exposure. When the duration of hydrogen exposure was over 90 min., we found that the surface was not oxidized. This was not due to bulk hydrogenation as demonstrated by our electron energy loss spectroscopy (EELS) results. We performed similar studies for the surface of platinum in oxygen after prolonged hydrogen exposure. However in platinum, the oxidation of the surface was not suppressed. This suggests that the process for suppression of oxidation, after prolonged hydrogen exposure, exists for palladium and not for platinum.

From these results, we hypothesize possible processes that explain how the prolonged hydrogen exposure suppresses the oxidation of palladium surface. We will also present atomic-scale in-situ movies on the surface dynamics in palladium and platinum in various processing.