Issue 25, 2007

Time-resolved in situXAS study of the preparation of supported gold clusters

Abstract

Incipient-wetness impregnation of γ-Al2O3 with HAuCl4 and subsequent removal of chlorine with NaOH, and deposition-precipitation of HAuCl4 on TiO2 at pH 7 resulted in supported Au3+ species. Time-resolved in situ XAS at the Au L3 edge showed that the Al2O3-supported oxidic or hydroxidic species were reduced in hydrogen at 440 K to yield small metallic gold clusters. The Au3+ precursor decomposed to metallic gold in inert atmosphere at 573 K and in oxidizing atmosphere above 623 K. In all atmospheres, initially small clusters were formed that gradually grew with increasing temperature. The TiO2-supported species were considerably less stable. In hydrogen and carbon monoxide, Au0 clusters of 1 to 1.5 nm were formed at room temperature, which was the lowest temperature studied. In inert and oxidizing atmosphere, the Au3+ precursor decomposed fully to metallic gold at 530 K, as shown by XAS and temperature-programmed experiments. Large clusters were obtained already in the initial stage of reduction. Residual chlorine inhibited the reduction and led to sintering of the gold clusters. Exposure of the TiO2-supported catalyst precursor to light or the X-ray beam led to partial reduction, and STEM showed that storage of the reduced gold clusters under ambient conditions led to agglomeration and bimodal cluster-size distributions.

Graphical abstract: Time-resolved in situ XAS study of the preparation of supported gold clusters

Article information

Article type
Paper
Submitted
22 Feb 2007
Accepted
19 Apr 2007
First published
04 May 2007

Phys. Chem. Chem. Phys., 2007,9, 3312-3320

Time-resolved in situ XAS study of the preparation of supported gold clusters

E. Bus, R. Prins and J. A. van Bokhoven, Phys. Chem. Chem. Phys., 2007, 9, 3312 DOI: 10.1039/B702747H

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Social activity

Spotlight

Advertisements