Surface activation inspires high performance of ultra-thin Pd membrane for 
hydrogen separation

Zhu, Bo; Tang, Chun H.; Xu, Heng Y.; Su, Dang Sheng; Zhang, Jian; Li, Hui

doi:10.1016/j.memsci.2016.12.025

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Surface activation inspires high performance of ultra-thin Pd membrane for hydrogen separation

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Su, Dang Sheng
Dalian Institute of Chemical Physics, Chinese Academy of Sciences;
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;
Institute of Metal Research, Chinese Academy of Sciences;

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Citation

Zhu, B., Tang, C. H., Xu, H. Y., Su, D. S., Zhang, J., & Li, H. (2017). Surface activation inspires high performance of ultra-thin Pd membrane for hydrogen separation. Journal of Membrane Science, 526, 138-146. doi:10.1016/j.memsci.2016.12.025.

Cite as: https://hdl.handle.net/11858/00-001M-0000-002D-7B32-D

Abstract

Pd-based membranes play a critical role in the field of hydrogen purification and small-scale hydrogen generation. The microstructure and composition of ultra-thin Pd membranes immediately determines their performance and stability, which are however complex and elusive. We applied for the first time a novel technique of environmental scanning electron microscopy (ESEM) together with EDS analysis for in-situ investigation of microstructure and composition of Pd composite membranes under gas-thermal treatment. It enables step by step analysis of the evolution process and offers more meticulous details compared to ex-situ technologies through analysis at exactly the same location of membrane samples. Here we observed the elimination of Pd crystallites as well as the homogenization/diffusion along the whole membrane surface following high T treatment under inert gas or H₂ atmosphere. Gradual evolution of microhillocks on Pd membrane surface was resulted due to α−β phase transition or exposure to either O₂ or H₂O, which can be effectively “smoothened” out during H₂ treatment. The exposure to steam exhibited a mild oxidation effect without pinhole formations, which appears a more appropriate surface cleaning process compared to air/oxygen treatment. A significant interlayer diffusion was revealed between Pd layer and ZrO₂/alumina substrate in H₂/O₂/H₂O atmosphere.