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Issue 24, 2016
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Restructuring of supported Pd by green solvents: an operando quick EXAFS (QEXAFS) study and implications for the derivation of structure–function relationships in Pd catalysis

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Abstract

Transmission electron microscopy (TEM) is commonly used as an ex situ technique to determine structural changes by comparing images of catalyst particles before and after a reaction. This requires the use of an alcoholic solvent to disperse the particles on a grid. In this work, we will show that Pd catalysts can be transformed during the procedure, by using EXAFS to determine the structure of Pd catalysts in different environments (as dry or wet samples). Supported palladium nanoparticles exposed to aqueous ethanolic solution (50% w/v) are transformed to a common, reduced, and hydrogen-contaminated state, irrespective of their initial habit or support. Catalysts comprised of nanosize PdO are reduced at ca. 350 K, whereas samples comprised of very small (ca. ≤10 atoms) Pd particles react with the solvent at just above room temperature and agglomerate with considerable loss of dispersion. As such any potential benefits to catalysis sought through the synthesis of very highly dispersed metallic Pd supported upon a range of inorganic dispersants will be rapidly erased through the action of such solvents.

Graphical abstract: Restructuring of supported Pd by green solvents: an operando quick EXAFS (QEXAFS) study and implications for the derivation of structure–function relationships in Pd catalysis

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Article information


Submitted
29 Sep 2016
Accepted
12 Nov 2016
First published
14 Nov 2016

This article is Open Access

Catal. Sci. Technol., 2016,6, 8525-8531
Article type
Paper

Restructuring of supported Pd by green solvents: an operando quick EXAFS (QEXAFS) study and implications for the derivation of structure–function relationships in Pd catalysis

M. A. Newton, J. B. Brazier, E. M. Barreiro, H. Emerich, L. A. Adrio, C. J. Mulligan, K. Hellgardt and K. K. (. Hii, Catal. Sci. Technol., 2016, 6, 8525
DOI: 10.1039/C6CY02073A

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