Journal of Colloid and Interface Science 475 (2016) 112118

Contents lists available at ScienceDirect

Journal of Colloid and Interface Science

journal homepage: www.elsevier.com/locate/jcis

Regular Article

Facet-selective photodeposition of gold nanoparticles on faceted ZnO

crystals for visible light photocatalysis
Xuewen Wang , Wuyou Wang, Yuanquan Miao, Gang Feng, Rongbin Zhang
The Institute of Applied Chemistry, The College of Chemistry, Nanchang University, 999# Xuefu Road, Nanchang 330031, PR China

g r a p h i c a l a b s t r a c t
The selective location of Au nanoparticles clearly confirms that polar facets sever as photoreductive sites in the photocatalyitc process.

Polar facet

Photoreductive
sites

a r t i c l e

i n f o

Article history:
Received 13 March 2016
Revised 29 April 2016
Accepted 29 April 2016
Available online 30 April 2016
Keywords:
ZnO
Polar facets
Gold
Plasmon
Photocatalysis
Visible light

a b s t r a c t
Hexagonal prism-like ZnO crystals dominated with polar facets were synthesized using a hydrothermal
method. The Gold (Au) nanoparticles were selectively photodeposited on the polar surfaces of faceted
ZnO crystals as a result of anisotropic photocatalytic activities of the polar and nonpolar facets. The size
of Au nanoparticles uniformly dispersed on the polar facets increased with increasing Au-loading
amount. These Au-loaded ZnO crystals showed an additional visible light absorption band from
400 nm to 800 nm. The 0.1 wt% Au-loaded ZnO crystals with visible light absorption peak at approximately 690 nm exhibited the highest photocatalytic activity under visible light irradiation.
2016 Elsevier Inc. All rights reserved.

1. Introduction

Corresponding authors.
E-mail addresses: wangxuewen@ncu.edu.cn (X. Wang), rbzhang@ncu.edu.cn
(R. Zhang).
http://dx.doi.org/10.1016/j.jcis.2016.04.048
0021-9797/ 2016 Elsevier Inc. All rights reserved.

Photocatalytic activity is sensitive to atomic structures on the

surface of semiconductors. Typical photocatalysts, such as TiO2,
Cu2O, BiVO4, BiOCl (Br), and ZnO, are dependent on the photocatalytic activity of the exposed facets [17]. TiO2 crystals bearing

X. Wang et al. / Journal of Colloid and Interface Science 475 (2016) 112118

different exposed facets have been widely studied for various

applications, including photodegradation, photocatalytic hydrogen
generation and solar cells [812]. Compared with TiO2 crystals
with surface comprising nonpolar facets, the surface of hexagonal
prism-like ZnO crystals consists of two top polar facets terminated
by Zn or O atoms and six lateral nonpolar facets terminated by Zn
and O atoms [2]. The unique atomic structure of polar facets renders these crystals with remarkable properties for controlling
ZnO based photocatalysts. Previous study demonstrated that photocatalytic hydrogen generation over the heterostructure of CdS
nanoparticle-modified ZnO crystals is related to the percentage
of the polar facets of ZnO used [2]. High percentage of polar facets
favors the activity of the catalyst. Selective deposition of photoactive modifiers on polar facets exhibits potential for improving photocatalytic activity.
Noble metal particles loaded on semiconductor photocatalysts
can improve photocatalytic activity by acting as electron collector
to promote separation and/or transfer of photogenerated charge
carriers [1315]. Some metals, such as Au and Ag, can increase visible light absorption as a consequence of surface plasmon resonance effect [9,10,1620]. Resonance wavelength depends on the
size and shape of metal particles, surface location, and interparticle
distance [2022]. Therefore, controlling the distribution of metal
nanoparticles on active crystal facets may result in multiple
enhancement. Au nanoparticles exhibit strong plasmon resonance
effect at wavelengths beyond 500 nm [10,2327]. In terms of Au
loading methods, the photodeposition using photogenerated electrons in photocatalysts for reducing Au species can control the
location of the Au product on the photocatalyst substrate.
In this study, ZnO crystals dominated with polar facets were
synthesized using a hydrothermal method. Au particles were selectively deposited on the polar facets of ZnO crystals through photoreduction. The plasmon resonance effect of Au significantly
contributes to visible light absorption of Au-loaded ZnO and photocatalytic activity to produce hydroxyl radicals under visible light
irradiation.
2. Experimental
2.1. Preparation of Au nanoparticle-loaded ZnO crystals
ZnO crystals dominated with polar facets were synthesized
using a hydrothermal method. Briefly, 0.02 mol zinc acetate [Zn
(CH3COO)2
2H2O] was dissolved in 50 mL of deionized water. Subsequently, 0.005 mol NaOH was added to the Zn(CH3COO)2 solution under magnetic stirring for 20 min. The white suspension
was hydrothermally treated in a 100 mL of Teflon-lined stainless
autoclave at 100 C for 10 h. The as-obtained white deposit, namely
ZnO crystals, was washed three times with deionized water and
dried at 100 C for 24 h. A predetermined quantity of H[AuCl4]
aqueous solution (Au: 1 mg mL 1) was added to 50 mL of aqueous
solution containing 200 mg of ZnO crystals under constant stirring.
Au nanoparticles were loaded on the surface of the ZnO crystals
through a photoreduction process under ultraviolet (UV) light irradiation (350 W Hg lamp) for 30 min. The crystals were washed
three times with deionized water and dried at 80 C for 24 h.
2.2. Characterization
X-ray diffraction (XRD) patterns were recorded by a Rigaku
diffractometer using Cu Ka irradiation. Scanning electron microscopy (SEM) images and energy dispersive X-ray (EDX) spectroscopy profiles were obtained on a Nova Nano 430.
Transmission electron microscope (TEM) images were obtained
by a JEOL-2100. The UVvisible absorption spectra were obtained

113

using a UVvisible spectrophotometer (JASCO-V550). The chemical

compositions of the samples were analyzed using a monochromatic Al Ka X-ray photoelectron spectroscopy (XPS) source
(Thermo Escalab 250). All binding energies were referenced to
the C 1s peak (284.6 eV) produced by adventitious carbon. Fluorescence spectra were obtained by a fluorescence spectrophotometer
(FLS920).
2.3. Photocatalytic activity measurement
The photocatalytic activity of the samples was determined in an
aqueous solution of terephthalic acid irradiated under different
wavelengths of light. Briefly, terephthalic acid solution was prepared using 1 L of deionized water, 0.5 g of terephthalic acid and
40 mg of NaOH. 50 mg of the sample was added to 100 mL of
3 mM aqueous solution of terephthalic acid. The mixed suspension
was stirred for 30 min in the dark to reach the adsorption equilibrium. Subsequently, 5 mL of the solution was sampled from the
suspension every 20 min (or 1 h) with constant magnetic stirring
under light irradiation. The solution was centrifuged to remove
the samples and then subjected to fluorescence spectroscopy
(FLS920). The excitation wavelength used in the fluorescence measurement was 325 nm. A Xe lamp (300 W) was used as the light
source of photocatalytic reaction. Long-pass and band-pass filters
were utilized to cut off the light.
3. Results and discussion
The ZnO crystals used in this study consisted of hexagonal
prism-like micron-sized crystals and synthesized through a
hydrothermal method (Fig. 1a). The crystal size of ZnO ranged from
1 lm to 10 lm. Two hexagonal surfaces at the top and bottom of

the particle are the polar surfaces that corresponded to (0 0 0 1)
and (0 0 0 1) facets of ZnO (Fig. 1b). The six lateral rectangular surfaces are nonpolar facets. The average percentage of polar facets in
the ZnO crystals is approximately 51%. The prepared ZnO crystals
dominated with polar facets render studies on anisotropic photocatalytic activity as possible.
Typical SEM images of the ZnO crystals loaded with 0.1 wt% Au
nanoparticles are shown in Fig. 2. The Au nanoparticle-loaded ZnO
crystals display a morphology similar to that of bare ZnO crystals.
SEM images (Fig. 2bd) clearly show the anisotropic distribution of
Au nanoparticles on the surface of the ZnO crystals. Au nanoparticles were predominantly located on the polar facets and occasionally observed on the nonpolar facets. During Au nanoparticle
loading, H[AuCl4] was reduced into Au nanoparticles through photogeneration of electrons from the active polar facets of the ZnO
crystal under UV light irradiation. These results clearly confirmed
that the polar facets of ZnO served as photoreductive sites during
photocatalysis.
Selective photodeposition of Au nanoparticles on the polar surface is independent of Au loading content. Fig. 3 shows the SEM
images of ZnO crystals loaded with 0.5 wt% Au nanoparticles.
SEM images of the local regions of the hexagonal prism-like ZnO
crystals in Fig. 3bf show that most Au nanoparticles are still predominantly located on the polar surface (the top and bottom facets
of the crystals). Selective Au deposition on the polar surface can be
well understood by considering the presence of dipole electric field
across the polar facets to promote the separation of photogenerated electrons and holes along the direction of electric fields. The
photogenerated electrons in ZnO under UV irradiation reached
the polar surface to induce the reduction of AuCl4 to form Au small
nanoparticles on the polar surface of ZnO. These small nanoparticles act as trapping sites for photoexcited electrons [15,2830] to
promote growth of Au nanoparticles on the polar surfaces.

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X. Wang et al. / Journal of Colloid and Interface Science 475 (2016) 112118

Fig. 1. (a) SEM image and (b) sketch map of hexagonal prism-like ZnO crystals.

Fig. 2. SEM images of (a) hexagonal prism-like ZnO crystals loaded with 0.1 wt% Au nanoparticles, and (bd) three local regions marked by squares in (a).

The plasmon resonance effect depends on size, shape and surface state [23,3136]. The morphology of the polar facets with different Au loading contents ranging from 0.05 wt% to 1 wt% was
determined to investigate the size and shape of Au nanoparticles
with increasing loading amount (Fig. 4). A 0.05 wt% Au-loading
(Fig. 4a) leads to the formation of a low-density of nanoparticles
on the polar facets. The TEM image in Fig. 4e suggests that the
average size of Au nanoparticles was approximately 9 nm in ZnO
loaded with 0.05 wt% Au. In the case of 0.1 wt% Au loading (Fig. 4b),
the density and size of Au nanoparticles on the facets increased.
Fig. 4b and f shows that the Au nanoparticles with an average particle size of approximately 14 nm were dispersed on the entire
facets. Moreover, aggregation of Au nanoparticles was not evident.
The EDX spectrum inset in Fig. 4c also suggests that the nanoparti-

cles loaded on the surface is Au. Au loading beyond 0.5 wt%

increased particle size because of the aggregation of primary
nanoparticles (Fig. 4c and d). The size of Au particles reached
100 nm at 0.5 wt% loading. Under 1 wt% Au loading, the nanoparticles agglomerated and formed large flower-like particles with a
size of approximately 200 nm.
The XRD patterns of ZnO crystals loaded with Au nanoparticles
are shown in Fig. 5. The major diffraction peaks of the samples are
consistent with those of the starting ZnO. The diffraction peaks of
Au were found between 37 and 47 (2h). The intensity of the
diffraction peaks of Au increased with increasing loading amount.
The broad XRD diffraction peaks of Au in all ZnO crystals with different Au loading amounts indicate that the Au nanoparticles
deposited in all samples exhibited similar size of primary crystal.

X. Wang et al. / Journal of Colloid and Interface Science 475 (2016) 112118

115

Fig. 3. SEM images of (a) ZnO crystals loaded with 0.5 wt% Au nanoparticles and (bf) five local regions marked by squares in (a).

Fig. 4. SEM images of the top surface of ZnO crystals loaded with (a) 0.05 wt%, (b) 0.1 wt%, (c) 0.5 wt%, and (d) 1 wt% Au nanoparticles. TEM images of ZnO crystals loaded
with (e) 0.05 wt% and (f) 0.1 wt% Au nanoparticles. The inset in (c) shows the EDX spectrum.

The chemical state of the loaded Au was investigated by XPS

(Fig. 6). The binding energies of Au 4d3/2 and 4d5/2 are
approximately 352.2 and 333.9 eV in 0.1 wt% Au-loaded ZnO
crystals, respectively, suggesting the formation of Au from the
photoreduction of H[AuCl4]. However, compared with substandard
binding energy, the slight shifts of the XPS peaks indicated
that Au-O and Au-Zn bonds were formed in the Au-loaded ZnO
crystals.
The UVvisible absorption spectra of ZnO crystals with different
amounts of Au loading are shown in Fig. 7a. Compared with ZnO

crystals, the Au-loaded ZnO crystals display an obvious additional

visible light absorption band. This band is attributed to the surface
plasmon resonance effect of Au nanoparticles [2124,33,37]
(Fig. 7b). Loading of 0.1 wt% Au resulted in a sharp absorption band
with the center located at approximately 690 nm. By contrast, the
light absorption bands caused by 0.5 wt% and 1 wt% Au loadings
are considerably broader, ranging from 400 nm to 800 nm. These
broad absorption bands could be largely attributed to aggregation
of primary Au nanoparticles into secondary particles with a wide
distribution of particle size.

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X. Wang et al. / Journal of Colloid and Interface Science 475 (2016) 112118

Au

Au

Intensity (a. u.)

Intensity (a. u.)

1%

0.5%

0.1%

ZnO
20

30

40

50

60

70

2 (degree)

80

38

40

42

44

46

2 (degree)

Fig. 5. Left panel: XRD patterns of ZnO crystals, ZnO crystals loaded with 0.1 wt%, 0.5 wt%, and 1 wt% Au nanoparticles. Right panel: The corresponding XRD patterns at 37
47 (2h) of those in the left panel.

Intensity (a. u.)

Au 4d

365

360

355

350

345

340

335

330

325

Binding Energy (eV)

Fig. 6. High-resolution XPS spectrum of Au 4d in 0.1 wt% Au-loaded ZnO crystals.

Hydroxyl radicals, an important active species in photocatalytic

reactions [38,39], can be generated by Au-loaded ZnO photocatalysts from an aqueous solution of terephthalic acid under visible
light irradiation (k P 420 nm). Fig. 8a shows the time-dependent

fluorescence emission spectra of 2-hydroxyterephthalic acid generated by reacting terephthalic acid with OH radicals in an aqueous suspension of ZnO crystals loaded with 0.1 wt% Au under
visible light irradiation. The continuous increase in the emission
peak centered at 426 nm with the increasing irradiation time suggested the generation of OH radicals. However, the fluorescence
intensity of the ZnO crystals (Fig. 8b) did not increase following
visible light irradiation for 1 h. This finding confirms that ZnO crystals without visible light absorption do not generate OH radicals.
The activity of ZnO loaded with 0.1 wt% Au under irradiation of
monochromatic lights at 450 and 700 nm was evaluated to determine the origin of the formation of OH radicals (Fig. 9a). The activity under the irradiation at 700 nm is considerably higher than that
under 450 nm. Fig. 9b and c shows the time-dependent fluorescence emission spectra of 2-hydroxyterephthalic acid generated
by reacting terephthalic acid with OH radicals in an aqueous suspension of 0.1 wt% Au-loaded ZnO crystals under monochromatic
light (450 or 700 nm) irradiation. The amount of OH radicals
increased with increasing light irradiation time under 700 nm; by
contrast, no photocatalytic activity was observed under 450 nm.
This finding is consistent with the strong absorption of Auloaded ZnO crystals at 700 nm; hence, the activity observed in
Fig. 8a is indeed caused by photocatalytic processes. Fig. 9d shows

1.0

(b)

(a)

ZnO

Absorbance / a. u.

0.8

e0.6
ZnO-Au-1

Au
ZnO

ZnO-Au-0.5

0.4

ZnO-Au-0.1
0.2
0.0
200

300

400

500

600

700

800

Wavelength / nm
Fig. 7. (a) UVvisible absorption spectra of ZnO crystals, ZnO crystals loaded with 0.1 wt%, 0.5 wt%, and 1 wt% Au nanoparticles. (b) Sketch map of plasmon resonance process
in Au-loaded ZnO crystals.

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X. Wang et al. / Journal of Colloid and Interface Science 475 (2016) 112118

1000

(a)

(b)

Au-loaded ZnO

2500

60 min

2000

40 min

1500

20 min

1000

0 min

60 min

800

Intensity (a. u.)

Intensity (a. u.)

3000

ZnO

40 min
600

20 min

400

0 min

200

500

400

450

500

550

390

420

450

480

510

540

Wavelength (nm)

Wavelength (nm)

Fig. 8. Time-dependent fluorescence emission spectra of (a) terephthalic acid aqueous solution over ZnO crystals loaded with 0.1 wt% Au nanoparticles and (b) ZnO crystals
irradiated by visible light irradiation (k P 420 nm). The excitation wavelength is 325 nm in the fluorescence measurement.

1200

1200

(a)

(b)

450 nm

1000

700 nm

800

Intensity (a. u.)

Intensity (a.u.)

1000

600

450 nm
400

800

3h

600

2h
400

200

200

1h
0 min

400

450

500

550

390

Wavelength (nm)

420

450

480

510

540

Wavelength (nm)

1200

(c)

3000

700 nm

1000

Intensity (a. u.)

Intensity (a.u.)

3h
800

2h
600

1h

400
200
0

(d)

2500
ZnO-Au-0.1

2000
ZnO-Au-0.5

1500
ZnO

1000
ZnO-Au-1

500

0 min

0
390

420

450

480

510

540

350

Wavelength (nm)

400

450

500

550

600

Wavelength (nm)

Fig. 9. (a) Fluorescence emission spectra of the terephthalic acid solution over ZnO crystals loaded with 0.1 wt% Au nanoparticles irradiated under 450 and 700 nm light for
1 h; time-dependent fluorescence emission spectra of the terephthalic acid solution over ZnO crystals loaded with 0.1 wt% Au nanoparticles irradiated under (b) 450 nm and
(c) 700 nm light; (d) fluorescence emission spectra of the terephthalic acid solution over ZnO and ZnO crystals loaded with 0.1 wt%, 0.5 wt%, and 1 wt% Au irradiated by visible
light (k P 420 nm) for 1 h. The excitation wavelength is 325 nm in the fluorescence measurement.

the comparison of the dependence of Au loading on photocatalytic

activity in generating OH radicals. Loading of 0.5 wt% Au reduced
the activity and 1 wt% Au further decreased the activity because
of the weak surface plasmon resonance effect caused by aggregated Au particles.

4. Conclusion
Au nanoparticles were selectively loaded on the polar facets of
ZnO crystals through photoreduction process under UV light irradiation. The selective location of Au nanoparticles clearly confirms

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X. Wang et al. / Journal of Colloid and Interface Science 475 (2016) 112118

that polar facets sever as photoreductive sites in the photocatalyitc

process, inducing the aggregation of photoexcited electrons and
holes on different facets. Plasmon resonance effects from Au
nanoparticles in the 0.1 wt% Au-loaded ZnO crystals generate an
absorption peak at approximately 690 nm under visible light. The
Au-loaded ZnO crystals developed in this work can generate a
number of OH radicals under visible light and 700 nm monochromatic light irradiation. This study provides insights into the photocatalytic reaction on the surface of ZnO.
Acknowledgement
The financial support from National Science Fund of China (No.
51202105), the Natural Science Foundation of Jiangxi Province
(20151BAB216006, 20122BAB203009), the Science and Technology Project of Education Department of Jiangxi Province, China
(No. GJJ14109), Opening Project of State Key Laboratory of High
Performance Ceramics and Superfine Microstructure (No.
SKL201205SIC). We also acknowledge great support from the Institute of Metal Research, Chinese Academy of Sciences.
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