Synthesis and characterization of structured interfaces for hydrogen generation. Study of an N,N′-dialkyl-4,4′-bipyridinium redox polymer/palladium catalyst system

James A. Bruce, Toshiaki Murahashi, Mark S. Wrighton

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92 Scopus citations

Abstract

Structured interfaces for H2 evolution have been synthesized and characterized. The substrates studied include W, Pt, and p-Si functionalized with N,N′-bis[3-(trimethoxysilyl)propyl]-4,4′-bipyridinium dibromide, I, to give polymeric quantities of a surface-confined N,N′-dialkyl-4,4′-bipyridinium (PQ2+) redox system, [(PQ2+)n]surf. (0.5 × 10-8-5 × 10-8 mol/cm2) with an Eo′ of -0.55 ± 0.05 V vs. SCE, in aqueous electrolyte solution. Incorporation of Pd(0) (<5 × 10-8 mol/cm2) into the substrate/[(PQ2+)n]surf system leads to improvement of H2-evolution kinetics for the W and p-Si electrodes. Various procedures have been used to prepare interfaces such as (i) substrate/Pd(0)/[(PQ2+)n]surf where Pd(0) coats the substrate and the [(PQ2+)n]surf is an overlayer, (ii) substrate/ [(PQ2+)n/Pd(0)]surf where the Pd(0) is only on the outermost surface, (iii) substrate/[(PQ2+-Pd(0))n]surf where the Pd(0) is dispersed throughout the polymer overlayer, and (iv) substrate/[(PQ2+)n/Pd(0)/(PQ2+) n]surf where the Pd(0) is sandwiched between two layers of polymer. Cathodes having no Pd(0) at the substrate/ [(PQ2+)n]surf interface equilibrate with H2O/H2 only via the [(PQ2+/·+)n]surf redox couple, whereas Pd(0) in direct contact with the substrate can equilibrate the substrate with H2O/H2. Interface structures have been synthesized by deliberate electrochemical procedures and have been confirmed by Auger depth profile analyses. Current-voltage properties for the cathodes have been used to correlate structure with the H2-evolution mechanism. Heavy metal impurity ions such as Hg2+ and Pb2+ have been identified as an important source of deactivation of the catalytic activity of Pd(0).

Original languageEnglish
Pages (from-to)1552-1563
Number of pages12
JournalJournal of Physical Chemistry
Volume86
Issue number9
DOIs
StatePublished - 1982

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