10
th
International Symposium “Scientific Bases for the Preparation of Heterogeneous Catalysts”
E.M. Gaigneaux, M. Devillers, S. Hermans, P. Jacobs, J. Martens and P. Ruiz (Editors)
© 2010 Elsevier B.V. All rights reserved.
Microwave-assisted synthesis of Au, Ag and Au-Ag
nanoparticles and their catalytic activities for the
reduction of nitrophenol
S. Albonetti
a
, M. Blosi
b
, F. Gatti
a
, A. Migliori
d
, L. Ortolani
d
, V. Morandi
d
, G.
Baldi
c
, A. Barzanti
c
, M. Dondi
b
a
Department of Industrial Chemistry and Materials, INSTM, Research Unit of Bologna,
Viale Risorgimento 4, 40136 Bologna University, Italy
b
ISTEC-CNR, Institute of Science and Technology for Ceramics, National Research
Council, Via Granarolo 64, 48018, Faenza, Italy
c
CERICOL, Via Pietramarina 123, 50053 Sovigliana Vinci, Firenze, Italy
d
IMM-CNR Sezione di Bologna - Via Gobetti, 101, 40129 Bologna, Italy
Abstract
A simple, microwave-assisted, strategy for producing Au/Ag concentrated sols by glucose
reduction in water was developed. PVP stabilized Ag-Au bimetallic nanoparticles were
characterized and their catalytic activity was studied in the reduction of 4-nitrophenol
with NaBH
4
as a probe reaction. The Ag-Au nanoparticles were prepared by first
optimizing the synthesis of Au colloid and then carrying out the deposition of a silver
shell. Microwave heating has been shown to provide more homogeneous particle
nucleation and shorter synthesis time than traditional heating. Prepared Au, Ag and
Au/Ag nanocrystals function as effective catalyst for the reduction of p-nitrophenol in the
presence of NaBH
4
otherwise unfeasible if only the strong reducing agent NaBH
4
is
employed.
Keywords: Au, Ag, microwave, bimetallic sols, nanoparticles, water media
1. Introduction
Colloidal suspension of different metals has found applications in various fields,
including catalysis, because a large fraction of the catalytically active metal sites in this
case is exposed to the reactants [1-2]. In particular, alloy and core-shell nanoparticles
have received special attention due to the possibility of tuning the optical and electronic
(and thus catalytic) properties over a broad range by simply varying the composition [3-
5].
2. Experimental procedure
2.1. Bimetallic synthesis
All the chemical reagents used in this experiment were analytical grade (Sigma Aldrich).
Au/Ag core-shell nanoparticles were prepared by a two-step method, characterized by the
shell synthesis on the preformed core used as seeds of nucleation (Scheme 1). Au-core
and Ag-core sols, exploited as seeds, were obtained separately through the reduction of
HAuCl
4
or AgNO
3
by glucose in alkaline water. PVP-coated metal seeds were
synthesized in 5 minutes at 70°C (for Ag) or at 90°C (for Au) by using microwave
heating and following a patented procedure [6]. For each metal, the glucose amount and
the solution pH were carefully optimized. Table 1 shows the characteristics corresponding