Synthesis, characterization, and testing of supported Au catalysts prepared from atomically-tailored Au38(SC12H25)24 clusters

Sarthak Gaur; Jeffrey T. Miller; Daniel Stellwagen; Ashwin Sanampudi; Challa S. S. R. Kumar; James J. Spivey

doi:10.1039/C1CP22438G

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Physical Chemistry Chemical Physics

Issue 5, 2012

High quality research in physical chemistry, chemical physics and biophysical chemistry.

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Synthesis, characterization, and testing of supported Au catalysts prepared from atomically-tailored Au₃₈(SC₁₂H₂₅)₂₄ clusters

Sarthak Gaur,^a Jeffrey T. Miller,^b Daniel Stellwagen,^c Ashwin Sanampudi,^a Challa S. S. R. Kumar^d and James J. Spivey*^a

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Cain Department of Chemical Engineering, Louisiana State University, 110 S. Stadium Dr, Baton Rouge, USA
E-mail: jjspivey@lsu.edu ;
Fax: 225-578-1476 ;
Tel: 225-578-3690

Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 South Cass Avenue, Bldg 200, Argonne, USA

Inorganic Chemistry and Catalysis, Debye Institute for Nanomaterials Science, Utrecht University, Universiteitsweg 99, Utrecht, The Netherlands

The J. Bennett Johnston Sr. Center for Advanced Microstructures and Devices, 6980 Jefferson Highway, Baton Rouge, USA

Phys. Chem. Chem. Phys., 2012,14, 1627-1634

DOI: 10.1039/C1CP22438G
Received 28 Jul 2011, Accepted 22 Sep 2011
First published online 17 Oct 2011

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Abstract
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Nearly monodispersed Au₃₈(SC₁₂H₂₅)₂₄ clusters (1.7 ± 0.2 nm) were synthesized using a modified Brust process while utilizing a “thiol etching” approach for the ligand exchange. HRTEM, MALDI, FTIR, and XAS analysis confirmed the formation of the 38-atom clusters in solution. This solution was used to impregnate a microporous TiO₂ support to give 0.7% Au₃₈/TiO₂ catalyst. Subsequent drying in air and treatment with H₂/He at 400 °C removed most of the sulfur ligands, and also increased the Au cluster size to 3.9 ± 0.96 nm. XPS and EXAFS analysis of this supported catalyst showed trace levels of residual sulfides, apparently located at the Au–TiO₂ interface. CO oxidation tests on these supported clusters show an activation energy and range of TOFs comparable to those reported by others. These results suggest that supported Au clusters of controllable size can be prepared with this thiol-ligated solution-based method, providing a new approach to the synthesis of these catalysts.

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Sarthak Gaur
Jeffrey T. Miller
Daniel Stellwagen
Ashwin Sanampudi
Challa S. S. R. Kumar
James J. Spivey

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Synthesis, characterization, and testing of supported Au catalysts prepared from atomically-tailored Au38(SC12H25)24 clusters

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Synthesis, characterization, and testing of supported Au catalysts prepared from atomically-tailored Au₃₈(SC₁₂H₂₅)₂₄ clusters