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Beilstein J Nanotechnol. 2014 May 28;5:735-46. doi: 10.3762/bjnano.5.86. eCollection 2014.

Shape-selected nanocrystals for in situ spectro-electrochemistry studies on structurally well defined surfaces under controlled electrolyte transport: A combined in situ ATR-FTIR/online DEMS investigation of CO electrooxidation on Pt.

Beilstein journal of nanotechnology

Sylvain Brimaud, Zenonas Jusys, R Jürgen Behm

Affiliations

  1. Institut für Oberflächenchemie und Katalyse, Ulm University, Albert-Einstein-Allee 47, D-89081 Ulm, Germany.

PMID: 24991511 PMCID: PMC4077536 DOI: 10.3762/bjnano.5.86

Abstract

The suitability and potential of shape selected nanocrystals for in situ spectro-electrochemical and in particular spectro-electrocatalytic studies on structurally well defined electrodes under enforced and controlled electrolyte mass transport will be demonstrated, using Pt nanocrystals prepared by colloidal synthesis procedures and a flow cell set-up allowing simultaneous measurements of the Faradaic current, FTIR spectroscopy of adsorbed reaction intermediates and side products in an attenuated total reflection configuration (ATR-FTIRS) and differential electrochemical mass spectrometry (DEMS) measurements of volatile reaction products. Batches of shape-selected Pt nanocrystals with different shapes and hence different surface structures were prepared and structurally characterized by transmission electron microscopy (TEM) and electrochemical methods. The potential for in situ spectro-electrocatalytic studies is illustrated for COad oxidation on Pt nanocrystal surfaces, where we could separate contributions from two processes occurring simultaneously, oxidative COad removal and re-adsorption of (bi)sulfate anions, and reveal a distinct structure sensitivity in these processes and also in the structural implications of (bi)sulfate re-adsorption on the CO adlayer.

Keywords: CO oxidation; Pt; electrocatalysis; in situ spectro-electrochemistry; shape selected nanocrystals

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