DOI: 10.1002/cctc.

201000380

Highly Efficient Visible Light Plasmonic Photocatalysts

Ag@Ag(Cl,Br) and Ag@AgCl-AgI
Peng Wang,[a] Baibiao Huang,*[a] Xiaoyang Zhang,[a] Xiaoyan Qin,[a] Ying Dai,[b] Zeyan Wang,[a]
and Zaizhu Lou[a]
New plasmonic photocatalysts Ag@Ag(Cl,Br) and Ag@AgCl-AgI
were synthesized by the ion-exchange process between AgCl
and a potassium halide (KBr, KI), then by reducing some Ag +
ions in the surface region of Ag(Cl,Br) and AgCl-AgI particles to
Ag0 species. The Ag nanoparticles were formed from Ag(Cl,Br)
and AgCl-AgI by a light-induced chemical reduction. The
Ag@Ag(Cl,Br) and Ag@AgCl-AgI particles have irregular shapes
and their sizes vary between 100 nm and 1.3 mm. The as-

grown plasmonic photocatalysts show strong absorption in

the visible-light region, owing to the plasmon resonance of Ag
nanoparticles. The ability of this compound to oxidize methylic
orange and reduce CrVI under visible light was compared with
those of other reference photocatalysts. These plasmonic photocatalysts have been shown to be highly efficient under visible-light irradiation.

Introduction
Since the first Ag@AgCl plasmonic photocatalyst was proposed,[12] plasmonic photocatalysts have attracted more and
more attention.[310] Unlike traditional photocatalysts,[1114] plasmonic photocatalysts are based on the localized surface plasmon resonance (LSPR) of the noble metal, metal-semiconductor contact, and semiconductor photocatalysts. The LSPR is essentially light waves trapped on the metal surface as a result
of the interaction with the free electrons of the metal.[1516] Excitation of the conduction electrons occurs when there is resonance between the electrons and the oscillating electric field
of the incident light, and this LSPR can be monitored as an extinction spectrum as light is passed through the sample. The
LSPR of metal nanoparticles can be modulated by their size,
shape, and surrounding medium.[1719] The plasmonic photocatalyst Ag@AgCl has proven to be a highly efficient and stable
photocatalyst under visible-light illumination. Based on the research of Ag@AgCl, we have changed the surrounding
medium of silver nanoparticles and succeed in fabricating the
new plasmonic photocatalysts Ag@Ag(Cl,Br) and Ag@AgCl-AgI.
By changing the surrounding medium, the photocatalytic performance and LSPR have been tuned.[20] The new plasmonic
photocatalysts Ag@Ag(Cl,Br) and Ag@AgCl-AgI are highly efficient for the photooxidization of methylic orange (MO) dye
and the photoreduction of CrVI.
The properties of Ag(Cl,Br) are similar to halide silver, but
Ag(Cl,Br) is seldom researched. Ag(Cl,Br) is also photosensitive
and can be decomposed by visible light. Just as AgCl, Ag(Cl,Br)
can also be used as a photocatalyst if photogenerated electrons are prevented from combining with Ag + ions.
Herein, we have synthesized the plasmonic photocatalysts
Ag@Ag(Cl,Br) and Ag@AgCl-AgI. The oxidative ability of the
plasmonic photocatalysts (photogenerated holes, degradation
of organic pollution) and reduction ability of the plasmonic
photocatalysts (photogenerated electrons, reducing CrVI) were

360

examined. The oxidative abilities of the plasmonic photocatalysts Ag@Ag(Cl,Br) and Ag@AgCl-AgI are stronger than N-TiO2.
The reducing ability of the plasmonic photocatalyst Ag@AgClAgI is stronger than N-TiO2, whereas the reducing ability of the
plasmonic photocatalyst Ag@Ag(Cl,Br) is weaker than N-TiO2.
The surrounding medium plays important role in the plasmonic performance of the photocatalysts. By changing the surrounding medium, the performance of the photocatalyst could
be tuned.

Results and Discussion

X-Ray diffraction and X-ray photoelectron spectroscopy
analysis of Ag@Ag(Cl,Br) and Ag@AgCl-AgI.
The XRD patterns of the obtained Ag@Ag(Cl,Br) and Ag@AgClAgI products are shown in Figure 1. Figure 1 a can be indexed
to the cubic phase of Ag (JCPDS file: 65-2871) coexisting with
the cubic phase of Ag(Cl,Br) (JCPDS file: 14-255). As seen from
Figure 1 b, all the diffractions can be indexed to the cubic
phase of Ag (JCPDS file: 65-2871), the cubic phase of AgCl
(JCPDS file: 31-1238), and the hexagonal phases of AgI (JCPDS
file: 9-374).
The elemental composition, chemical status, and silver content of Ag@Ag(Cl,Br) and Ag@AgCl-AgI were also examined by
X-ray photoelectron spectroscopy (XPS). Before the visible-light
[a] Dr. P. Wang, Prof. Dr. B. Huang, Prof. X. Zhang, X. Qin, Dr. Z. Wang, Z. Lou
State Key Lab of Crystal Materials, Shandong University
Jinan 250100 (China)
Fax: (+ 86) 531-8836-5969
E-mail: bbhuang@sdu.edu.cn
[b] Prof. Dr. Y. Dai
School of Physics, Shandong University
Jinan 250100 (China)

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Silver Visible Light Plasmonic Photocatalysts

ples was also calculated. The content of Ag0 of the as-obtained
Ag@AgCl-AgI (3.31 mol %) was also calculated from XPS data
(not shown here). The spectra of Cl 2p and Br 3d are shown in
Figure 3, the binding energies of Cl 2p1 and Cl 2p3 are 199.40
and 197.75 eV, and the binding energies of Br 3d3 and 3d5 are
69.26 and 68.20 eV. The calculated surface content values for
Cl and Br are 16.41 and 28.47 mol %, respectively.

Electron microscopy analysis and UV/Vis diffuse reflectance

spectra of Ag@Ag(Cl,Br) and Ag@AgCl-AgI.

Figure 1. The XRD patterns of a) Ag@Ag(Cl,Br) and b) Ag@AgCl-AgI.

The scanning electron microscopy (SEM) images of Figure 4

show the morphologies of the as-prepared Ag@Ag(Cl,Br) and
Ag@AgCl-AgI samples. The size of the Ag@Ag(Cl,Br) (100 nm
1 mm, Figure 4 a) and Ag@AgCl-AgI (165 nm1.3 mm, Figure 4 b)

irradiation, XPS results indicated that the Ag@Ag(Cl,Br) contained Ag, Cl, Br, and C elements. The C element was attributed to adventitious hydrocarbon from the XPS instrument itself.
The Ag, Cl and Br peaks were attributed to the as-obtained
Ag@Ag(Cl,Br) samples. Shown in Figures 2 and 3 are the XPS
spectra of Ag@Ag(Cl,Br). The binding energy values taken from
Figure 4. SEM images of a) Ag@Ag(Cl,Br) and b) Ag@AgCl-AgI samples.

Figure 2. XPS spectra of Ag 3d in Ag@Ag(Cl,Br) samples.

particles could also be calculated from the SEM images. The

size and position of the Ag nanoparticles was difficult to confirm. Higher resolution images could be achieved because Ag(Cl,Br) and AgCl-AgI were decomposed under the high energy
electron beam.
The UV/Vis diffuse reflectance spectra of Ag@Ag(Cl,Br),
Ag@AgCl-AgI, Ag@AgCl, and N-TiO2 are presented in Figure 5.
The absorption in the UV and visible-light region was very
good for Ag@Ag(Cl,Br), Ag@AgCl-AgI, and Ag@AgCl, which all
exhibit stronger absorption in the visible region than N-TiO2.
Owing to the different surrounding medium of silver nanoparticles, the spectra of the plasmonic photocatalysts were different from each other; Ag@Ag(Cl,Br) shows the weakest absorp-

Figure 3. XPS spectra of a) Cl 2p and b) Br 3d of the as-obtained Ag@Ag(Cl,Br) samples.

the XPS spectra were calibrated by using C 1s (284.8 eV). In Figure 2 a, the Ag 3d spectra of Ag@Ag(Cl,Br) consists of two individual peaks at 373 and 367 eV, which were attributed to
Ag 3d3/2 and Ag 3d5/2 binding energies, respectively. The
Ag 3d3/2 and Ag 3d5/2 peaks can be further divided in two,
373.64, 374.11 eV, and 367.65 eV, 368.49 eV, respectively. The
peaks at 374.11 and 368.49 eV were attributed to metal Ag0,
whereas the peaks at 367.65 and 373.64 eV were attributed to
AgI of Ag(Cl,Br). The surface Ag0 content (4.13 mol %) and the
surface Ag + content (51.00 mol %) of the corresponding samChemCatChem 2011, 3, 360 364

Figure 5. UV/Vis diffuse reflectance spectra of the photocatalysts:

a) Ag@AgCl, b) Ag@AgCl-AgI, c) Ag@Ag(Cl,Br), and d) N-TiO2.

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www.chemcatchem.org

361

B. Huang, Z. Lou et al.

tion in visible-light region, whereas Ag@AgCl shows the strongest absorption in visible-light region.

Photocatalytic activities of Ag@Ag(Cl,Br) and Ag@AgCl-AgI.

The photooxidation capabilities of the Ag@Ag(Cl,Br) and
Ag@AgCl-AgI samples were evaluated by measuring the decomposition of methylic orange (MO) dye in solution (concentration = 20 mg L 1) under visible-light irradiation. Shown in
Figure 6 is the degradation rate of MO over different photoca-

Figure 6. Photodecomposition of MO dye in solution (20 mg L 1) over

Ag@Ag(Cl,Br) and Ag@AgCl-AgI under visible-light irradiation (l  400 nm). C
is the concentration of MO dye at time t, and C0 that in the MO solution immediately after it is kept in the dark to obtain equilibrium adsorption state.

talysts. Prior to visible-light irradiation, the MO solution over

the catalyst was kept in the dark for 30 min to reach an equilibrium adsorption state. The concentration of the MO solution
slightly decreased as it was kept in the dark; C0 is the equilibrium concentration of MO after equilibrium adsorption state,
and C is the concentration of MO after visible-light irradiation.
A blank experiment in the absence of the photocatalyst, but
under visible-light irradiation, showed that no MO decomposed. Another blank experiment without irradiation, using
Ag@Ag(Cl,Br) and Ag@AgCl-AgI as the photocatalysts, demonstrated that the concentration of MO remained unchanged.
The MO solution was decolorized completely by using Ag@Ag(Cl,Br) after exposure to visible-light irradiation for 15 min
(Figure 6). As shown in Figure 6, about 90 percent of the MO
had decomposed after exposure for 25 min over the Ag@AgClAgI photocatalyst. Provided that the reaction follows a
pseudo-first order reaction, the rate of MO decomposition over
Ag@Ag(Cl,Br) is estimated to be about 0.133 mg min 1 (equal
to the rate over Ag@AgCl), faster than that over Ag@AgCl-AgI (
 0.072 mg min 1). The rates over the Ag@Ag(Cl,Br) and
Ag@AgCl-AgI plasmonic photocatalysts are faster than that
over N-doped TiO2 (  0.017 mg min 1).[1]
CrVI can be reduced to CrIII by photocatalytic reduction,[2123]
the mechanism of which has been reported many times.[2425]
Shown in Figure 7 a is the photocatalytic reduction of CrVI over
the plasmonic photocatalyst Ag@AgCl-AgI, which exhibited a
high photocatalytic activity for CrVI reduction under visible
light. The concentration of CrVI decreased with increasing irra-

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Figure 7. a) Changing UV/Vis spectrum of the aqueous solution in the presence of Ag@AgCl-AgI under visible-light irradiation. (using diphenycarbazide
as a developer at l = 540 nm) b) Photocatalytic reduction of CrVI in a slurry
system over plasmonic photocatalysts Ag@Ag(Cl,Br), Ag@AgCl-AgI,
Ag@AgCl, and N-TiO2 under visible-light irradiation (l  400 nm). C is the
concentration of CrVI at time t, and C0 that in the slurry system immediately
after it is kept in the dark to obtain equilibrium adsorption state.

diation time and nearly half the amount of CrVI was photoreduced after only 5 min irradiation; almost all of the CrVI was reduced to CrIII after irradiation for 10 min. Shown in Figure 7 b is
the photocatalytic reduction of CrVI over Ag@Ag(Cl,Br),
Ag@AgCl-AgI, Ag@AgCl, and N-TiO2. The results indicate that
the rate of CrVI reduction with the Ag@AgCl-AgI as a photocatalyst was faster than that with Ag@Ag(Cl,Br), N-TiO2, or
Ag@AgCl. Blank experiments in the absence of the photocatalyst, but under visible-light irradiation, and blank experiments
using Ag@Ag(Cl,Br) and Ag@AgCl-AgI without irradiation, demonstrated that the concentration of CrVI remained unchanged.
The plasmonic photocatalysts Ag@Ag(Cl,Br) and Ag@AgClAgI can be used to decompose organic pollution, such as our
example methylic orange (MO), and reduce CrVI. By varying the
surrounding medium, plasmonic photocatalysts can show different efficiency in decomposing MO and reducing CrVI. During
the process of the destruction of MO, the amount of photogenerated holes that transfer to the surface of the system corresponds to the oxidation of the MO dye. The photogenerated
electrons are likely trapped by O2 in solution to form superoxide ions and other reactive oxygen species.[26] During the process of CrVI decay, the photogenerated electrons correspond to
the reduction of CrVI. The photogenerated holes were expected
to be trapped by EDTA.[24] The activities of the photogenerated

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Silver Visible Light Plasmonic Photocatalysts

electrons and photogenerated holes determined the reduction
and oxidative abilities of the photocatalysts, respectively. From
the photocatalytic reaction, we found that the oxidative ability
of Ag@Ag(Cl,Br) was stronger than that of Ag@AgCl-AgI,
whereas the reducing power of Ag@Ag(Cl,Br) was weaker than
that of Ag@AgCl-AgI. Compared with the traditional photocatalysts, the plasmonic photocatalysts show outstanding activities, owing to the strong absorption of visible light (surface
plasmon resonance of silver nanoparticles) and effective separation of the photogenerated electrons and holes (good surface contact of Ag metal particles to the semiconductors). The
performance of the plasmonic photocatalysts can be tuned by
changing the surrounding medium of silver nanoparticles.

Conclusions
Plasmonic photocatalysts Ag@Ag(Cl,Br) and Ag@AgCl-AgI have
been fabricated by a simple ion-exchange process and light-induced chemical reduction. The photocatalysts have strong absorption in the visible-light region for the plasmon resonance
of Ag nanoparticles. The plasmonic photocatalysts show highly
efficiency in reduction of CrVI and degradation of MO under
visible-light irradiation. The study on plasmonic photocatalysts
Ag@Ag(Cl,Br) and Ag@AgCl-AgI strongly suggests that the performance of the plasmonic photocatalysts and the LSPR of the
noble metals can be tuned by changing the medium surrounding the noble metal nanoparticles.

Experimental Section
Preparation of AgCl: Silver molybdate was synthesized as previously described.[1] AgCl was synthesized by the ion-exchange reaction
between the prepared silver molybdate and HCl. Ag2MoO4 was sonicated in concentrated HCl until completion of the ion-exchange
process. The precipitated AgCl was collected, washed with deionized water, and dried in air.
Preparation of Ag@Ag(Cl,Br) and Ag@AgCl-AgI: AgCl (1.432 g) was
added into the reaction vessel, which contained a solution of KBr
(100 mL, 0.05 mol L 1, and KI). The vessel was stirred for about 3
5 days. The Ag(Cl,Br) and AgCl-AgI precipitate was then collected,
washed with deionized water and dried in air.
The as-obtained Ag(Cl,Br) and AgCl-AgI powders were put into a
solution of MO dye, which was then irradiated with a 300 W Xe arc
lamp equipped with an ultraviolet cutoff filter to provide visible
light with l  400 nm. The resulting precipitates, which consist of
silver NPs and Ag(Cl,Br), AgCl-AgI particles, were then washed and
dried in air.
The crystal structures of the samples were examined by using Xray diffraction (XRD, Bruker AXS D8), their morphology by using
scanning electron microscopy (SEM, Hitachi S-4800 microscopy),
and their diffuse reflectance by using UV/Vis spectroscopy (UV2550, Shimadzu). The content of Ag element in Ag(Cl,Br) and AgClAgI photocatalysts was confirmed by using X-ray photoelectron
spectroscopy measurements (VG MicroTech ESCA 3000 X-ray photoelectron spectroscope using monochromatic A1Ka with a photon
energy of 1486.6 eV at a pressure of > 1  10 9 Torr, a pass energy
of 40 eV, an electron takeoff angle of 60 8C, and an overall resolution of 0.05 eV). The XPS spectra were fitted by using a combined
ChemCatChem 2011, 3, 360 364

polynomial and Shirley-type background function. A reference

photocatalyst, N-doped TiO2, was prepared by nitridation of commercially available TiO2 powder (with a surface area of 50 m2 g 1) at
773 K for 10 h under NH3 flow (flow rate of 350 mL min 1).[27]
Evaluation of photocatalytic activities: The activities of the photocatalysts were evaluated by studying the degradation of methylic
orange (MO) dye and reduction of CrVI. The photocatalytic degradation of MO dye was performed with Ag@Ag(Cl,Br) and Ag@AgClAgI (0.2 g) photocatalysts suspended in a solution of MO dye
(100 mL, 20 mg L 1). The degradation of MO dye was monitored by
using UV/Vis spectroscopy (UV-7502PC, Xinmao, Shanghai). The reduction of the CrVI was performed with Ag@Ag(Cl,Br) and
Ag@AgCl-AgI (0.1 g) photocatalysts suspended in a solution of
K2CrO4 (100 mL, 14.24 mg L 1). The pH of the reaction suspension
was adjusted to 2 with dilute HClO4, and the ethylene diamine tetraacetic acid (EDTA) has also been added as sacrificial reagent.
After the photocatalytic experiment was started by the irradiation
of visible light, 5 mL aliquots were periodically withdrawn from the
reaction vessel, and the CrVI concentration was measured by using
the diphenycarbazide (DPC) method at l = 540 nm[2829] by using a
UV/Vis spectrophotometer (UV-7502PC, Xinmao, Shanghai). The optical system for detecting the catalytic reaction included a 300 W
Xe arc lamp (PLS-SXE300, Beijing Trusttech Co. Ltd) with UV cutoff
filter (providing visible light l  400 nm).

Acknowledgements
This work was financially supported by the National Basic Research Program of China (973 Program, Grant 2007CB613302),
the National Natural Science Foundation of China under Grant
50721002, 20973102 and 10774091 and China Postdoctoral Science Foundation under Grant 20090461200.
Keywords: catalysis photocatalysis photochemistry
plasmon silver
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Received: October 27, 2010

Published online on January 3, 2011

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ChemCatChem 2011, 3, 360 364