Fabrication of an Ag/Fe2O3/ZnO ternary composite with enhanced photocatalytic performance

Article abstract of DOI:10.1039/c5ra20403h

A novel Ag/Fe₂O₃/ZnO ternary composite was fabricated using the chemical deposition and photochemical deposition methods. Its structure and optical properties were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and ultraviolet-visible spectrophotometry. The Ag/Fe₂O₃/ZnO ternary composite exhibited a greater improvement in photocatalytic activity compared with the Fe₂O₃/ZnO or Ag/ZnO binary composite. The degradation rate of Ag/Fe₂O₃/ZnO towards methyl orange (MO) and iodoform (CHI₃) within 120 min was 80% and 94%, respectively. More importantly, the Ag/Fe₂O₃/ZnO composite had a much higher degradation efficiency towards iodoform, which indicates its efficient and selective degradation characteristics. The results show that the Ag/Fe₂O₃/ZnO ternary composite holds great potential in the removal of carcinogenic iodoform from sewage.

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Paper
Fabrication of Ag/Fe2O3/ZnO Ternary Composite with
Enhanced Photocatalytic Performance
Received 00th January 20xx,
Accepted 00th January 20xx
Jia-gen Wu‡, Ting Fang‡, Ran Cai, Shao-yang Li, Yue Wang, Cui-e Zhao and Ang Wei *
DOI: 10.1039/x0xx00000x
A novel Ag/Fe2O3/ZnO ternary composite was fabricated by chemical deposition and photochemical deposition methods.
The structure and optical properties were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM),
transmission electron microscopy (TEM) and ultraviolet-visible spectrophotometer. The Ag/Fe2O3/ZnO ternary composite
exhibited a greater improvement in photocatalytic activity compared with Fe2O3/ZnO or Ag/ZnO binary composite. The
degradation rate of Ag/Fe2O3/ZnO towards methyl orange (MO) and iodoform (CHI3) within 120 min was 80% and 94%,
respectively. More importantly, the Ag/Fe2O3/ZnO had much higher degradation efficiency towards iodoform, indicating
the efficient and selective degradation characteristics. The results show that the Ag/Fe2O3/ZnO ternary composite holds
great potential in removing of carcinogenic iodoform from sewage.
www.rsc.org/
defects. It cannot selectively photodegrade some hazard
1. Introduction
pollutants
in
wastewater,
especially
halogenated
hydrocarbons. Furthermore, the degradation efficiency
decreases obviously when there is a variety of pollutants in
wastewater. Recent studies have found that ZnO-based
ternary composites have great superiority than binary
composites 7, 8. Besides, they have the function of selective
Environment and human health are now threatened by a lot of
pollutants in wastewater. The harm is still so great despite of
the presence of low amount of halogenated hydrocarbon in
wastewater, for example, iodoform that can even cause cancer
1-3. Thus the removal of such toxic organic pollutants in
9
degradation of some pollutants . Also, it has been found that
wastewater is
a highly essential issue. Semiconductor
Ag has a strong adsorption of high carcinogenic halogenated
hydrocarbon 10
photocatalysts such as TiO2 and ZnO can be a green and
efficient technology in the field of sewage treatment, because
they can effectively dispose many organic pollutants in the
sewage compared with other approaches. Additionally, most
.
In this work, the Ag/Fe2O3/ZnO ternary composite was
synthesized by chemical deposition and photochemical
deposition process. The photocatalytic activity of
Ag/Fe2O3/ZnO was investigated in comparison with Fe2O3/ZnO
or Ag/ZnO. Furthermore, the effects of structure and
interfacial electronic interactions among ZnO, Fe2O3 and Ag on
the photocatalytic activity were also investigated. The
photocatalytic materials are non-toxic, stable and low-cost 4, 5
.
Although ZnO have a lot of advantages such as high
quantum efficiency, non-toxic and strong ultraviolet
absorption 6, its catalytic efficiency is still unideal. The main
reasons include: (1) The band gap of ZnO is too wide, only the
ultraviolet part of the sun light can be used; (2) ZnO is
amphoteric oxide semiconductor, it easily dissolved in strong
acid and alkali solution; (3) The electron-hole pairs in ZnO are
easy to recombine, which reduces the photocatalytic
efficiency. In this regard, combining ZnO with other metal
compounds such as CuO and Fe2O3 has been proved to be
effective in improving the photocatalytic performance of ZnO.
However, ZnO binary composite materials also have some
Ag/Fe2O3/ZnO
ternary
composite
had
effective
photodegradation toward MO and iodoform under irradiation
of simulated daylight, and it had higher degradation efficiency
towards iodoform. The results indicated the potential
applications of Ag/Fe2O3/ZnO in sewage treatment.
2. Experiments
2.1 Preparation of the Ag/Fe2O3/ZnO ternary composite
Key Laboratory for Organic Electronics and Information Displays & Institute of
Advanced Materials (IAM), Jiangsu National Synergetic Innovation Center for
Firstly, ZnO seed layer was prepared by a sol-gel method.
Briefly, 40 ml anhydrous ethanol, 0.5 M zinc acetate-2-hydrate,
Advanced Materials (SICAM), Nanjing University of Posts
&
and 0.5 M ethanol amine were mixed, and stirred at 70
℃for
Telecommunications, 9 Wenyuan Road, Nanjing 210023, China.
3 h. The resultant sol was transparent. The solution was then
spin-coated on the glass substrate at 500 rpm for 10 s and
*Correspondence author. Email: wei1177@126.com
‡ These authors contributed equally to this work.
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3000 rpm for 30 s, respectively. After that, the glass substrate
was heated at 300°C for 2h to remove the solvent.
Subsequently, the growth of ZnO nanorod (NR) was carried out
by suspending the glass substrate in a 40 mL beaker that filled
with an equimolar aqueous solution of 0.1 M zinc nitrate
3. Result and Discussion
3.1 Characterization of materials
Fig. 1 shows the XRD pattern of the as-prepared sample. The
typical diffraction peaks (0 0 2), (1 0 2), (1 1 0), (1 0 3), (2 0 1)
of hexagonal wurtzite ZnO are observed, which are in good
agreement with standard patterns (JSPDSNO.36-1451). In
addition, three diffraction peaks (2 0 6), (2 1 12), (5 2 1)
(JCPDSNO.13-0458) of Fe2O3 and four diffraction peaks (2 2 0),
(3 1 1), (3 3 1), (4 2 0) (JSPDSNO.01-1164) of Ag are observed,
revealing that the obtained Ag/Fe2O3/ZnO ternary composite
has good crystalline structure.
hexahydrate (Zn(NO3)2·6H2O), and 0.1
(C6H12N4 , HMT) at 75 °C for 3 h 11, 12
M methenamine
.
Fe2O3 nanoparticles were then deposited on the ZnO
nanorod by photochemical deposition. The ZnO nanorods-
coated substrate was immersed in a mixture of 4 mM
FeCl3·6H2O and NaNO3·6H2O aqueous solution, and then
irradiated with UV light for 1 h (wavelength 365 nm, power 56
W, working distance 0.3 m) 13, 14
.
Ag nanoparticles were further prepared by photochemical
deposition. Fe2O3/ZnO nanorods-coated substrate was
immersed in a 1 mM AgNO3 and NaNO3·6H2O aqueous
solution, and then irradiated with UV light (wavelength 365
nm, power 56 W, working distance 0.3 m) at room
temperature for 40 min. The prepared sample was post-
annealed in ambient air at 400
structure.
℃for 2 h to obtain the crystal
2.2 Characterization
The crystal structure of the products was characterized by X-
ray diffraction (XRD , Siemens D5005). The scanning electron
microscopy (SEM, S4800) was employed to investigate the
morphology. Transmission electron microscopy (TEM), high-
resolution electron microscopy (HRTEM) and selected area
electron diffraction (SAED) were measured with a Tecnai G2
F20 S-TWIN. The UV–vis absorption spectra were analyzed by
UV-2401PC spectrometer.
Fig. 1 The XRD patterns of the Ag/Fe2O3/ZnO ternary composite.
The as-prepared samples are characterized by SEM. As
shown in Fig. 2a, it is obvious that the wurtzite ZnO rods are
hexagonal structure, and the surface is relatively smooth (Fig.
2a inset). Under the irradiation with UV light, the Fe2O3
nanoparticles are coated on the surface of ZnO to form
Fe2O3/ZnO binary composite (Fig. 2b), resulting in a rough
layer on the nanorods (Fig. 2b inset). After the decoration of
Ag nanoparticles, the granular materials are observed on the
surface of Fe2O3/ZnO (Fig. 2c and 2c inset), indicating the
formation of the Ag/Fe2O3/ZnO ternary composite.
2.3 Photocatalytic studies
Iodoform
（halogenated hydrocarbon）and MO (organic dye)
are two common pollutants in wastewater. Iodoform and MO
were chosen to investigate the photo-degratation
characteristic of Ag/Fe2O3/ZnO ternary composite, Fe2O3/ZnO
and Ag/ZnO binary composite. Samples were put in 30 ml of
iodoform solution (1.65 mmg/L) and MO solution (6.67
mmg/L) with irradiation of simulated sunlight (xenon lamp,
wavelength 320-780 mm, the light intensity at the sample is
about 50 mW/cm2), respectively. The solutions of iodoform
and MO were taken every 30 min to analyze their ultraviolet
absorbance, respectively.
To investigate the reusability of Ag/Fe2O3/ZnO ternary
composite, the Ag/Fe2O3/ZnO modified glass substrates were
put into 30 ml of iodoform solution (1.65 mmg/L) and MO
solution (6.67 mmg/L) under irradiation of simulated sunlight
for 5 cycles, respectively. Each cycle, the iodoform and MO
solutions were degraded by Ag/Fe2O3/ZnO for 120 min and
measured their maximum absorbance, respectively. In the
next cycle, replacing the solutions of iodoform and MO, the
same Ag/Fe2O3/ZnO modified glass substrates were used again
to degrade iodoform and MO for 120 min and measured their
maximum absorbance, respectively.
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Fig. 2 SEM images of (a) ZnO nanorod arrays, (b) Fe2O3/ZnO binary composite, and (c)
Fe2O3 (Fig. 4b). Likewise, with the continued UV irradiation,
more and more Fe2O3 particles are obtained, leading to a thick
layer covered on the surface of ZnO (Fig. 4c). Finally, in
aqueous solution of AgNO3 and NaNO3·6H2O, Ag+ and OH- were
deposited on the surface of Fe2O3/ZnO, generating nanosized
silver particles 17 (Fig. 4d).
Ag/Fe2O3/ZnO ternary composite.
To further clarify the structure and morphology of
Ag/Fe2O3/ZnO ternary composite, HRTEM was performed. As
shown in Fig. 3a, it is noted that the product is hierarchical
structures. The high-magnification image of Fig. 3a (indicated
by the white rectangle) suggests that the lattice spacing is
about 0.248 nm, 0.155 nm and 0.144 nm (Fig. 3b),
corresponding to the (1 0 1) plane of ZnO, the (5 2 1) plane of
Fe2O3, and the (2 2 0) plane of Ag, respectively. The data
indicates the existence of ZnO, Fe2O3 and Ag in the composite.
The corresponding selected area electron diffraction (SAED)
patterns further confirm the successful formation of
Ag/Fe2O3/ZnO ternary composite (Fig. 3c).
Fig.
4 The proposed growth model of Ag/Fe2O3/ZnO ternary composite, (a) ZnO
nanorods were grown on the substrate of glass, (b) Fe2O3 nanoparticles were attached
to the surface of ZnO, (c) the Fe2O3 layer was coated on the surface of ZnO, and (d) Ag
nanoparticles were uniformly deposited on the surface of Fe2O3/ZnO to form the
Ag/Fe2O3/ZnO ternary composite.
3.3 Photocatalytic activity
Fig. 5 shows UV–vis absorption spectra of Ag/ZnO, Fe2O3/ZnO
and Ag/Fe2O3/ZnO, respectively. Remarkably, the absorption
wavelength of Ag/Fe2O3/ZnO ternary composite is up to 650
nm, which is much wider than that of Ag/ZnO or Fe2O3/ZnO.
The result indicates that the Ag/Fe2O3/ZnO can improve the
absorption intensity in the visible region. Therefore, the
Ag/Fe2O3/ZnO ternary composite has great potential in terms
of light degradation.
Fig. 3 (a) TEM image of the Ag/Fe2O3/ZnO ternary composite, (b) HR-TEM image of the
area indicated by white rectangle in (a), and (c) the SAED pattern of (a).
3.2 Growth mechanism
Fig. 5 UV–vis absorption spectra of Ag/ ZnO, Fe2O3/ZnO and Ag/Fe2O3/ZnO.
The proposed growth mechanism of Ag/Fe2O3/ZnO ternary
composite is shown in Fig. 4. Firstly, with the addition of HMT
and Zn(OH)42-, the ZnO rod arrays were coated on the glass
The photodegrade efficiency of Fe2O3/ZnO, Ag/ZnO, and
Ag/Fe2O3/ZnO under illumination and without illumination (Fig.
S1) were investigated. To calculate the concentration of the
iodoform and MO solutions, the solutions were collected every
30 min and measured the absorption intensity at their
maximum absorbance wavelength, respectively. Fig. 6 shows
UV-vis absorption spectra of iodoform and MO degraded by
substrate with ZnO seed layer under hydrothermal treatment
15
at 75
℃
(Fig. 4a). Secondly, under UV irradiation, ZnO could
form electronic-hole pairs. As a result, a great deal of OH- and
Fe3+ were deposited on the surface of ZnO nanorod to form
[Fe(OH)4]- ions, and then they removed OH− and H2O to form
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Fe2O3/ZnO, Ag/ZnO, and Ag/Fe2O3/ZnO, respectively. When iodoform, MO and RhB was 89%, 45% and 40% (Fig. S2),
Ag/ZnO was used as the photocatalyst materials, the respectively. The data indicated that the Ag/Fe2O3/ZnO
characteristic absorption peaks of iodoform and MO dropped exhibited a greater improvement in photocatalytic activity
to about 44% and 50% of their initial absorption intensity after compared with Fe2O3/ZnO or Ag/ZnO. More importantly, the
120 min (Fig. 6a), respectively. As for Fe2O3/ZnO, the results also suggested that the Ag/Fe2O3/ZnO ternary
absorption peaks of iodoform and MO reduced to about 40% composite had efficient and selective degradation towards
of their initial absorption intensity after 120 min (Fig. 6b), iodoform.
respectively. Interestingly, when the Ag/Fe2O3/ZnO was used,
the absorption peaks of iodoform and MO rapidly decreased to
about 5% and 22% of their initial intensity after 120 min,
respectively (Fig. 6c). Obviously, the Ag/Fe2O3/ZnO ternary
composite had much higher degradation efficiency towards
iodoform and MO compared to Ag/ZnO or Fe2O3/ZnO.
Fig.
7 Photo-degradation efficiency of iodoform and MO under illumination. The
degradation curve of Ag/Fe2O3/ZnO for iodoform (curve 1), and for MO (curve 2), the
degradation curve of Fe2O3/ZnO for MO (curve 3), and for iodoform (curve 4) , the
degradation curve of Ag/ ZnO for iodoform (curve 5), and for MO (curve 6).
3.4 The reusability of Ag/Fe2O3/ZnO composite
To examine the reusability of Ag/Fe2O3/ZnO ternary composite,
it was used as the photocatalysts material for 5 cycles. The
iodoform and MO solutions were replaced every 120 min and
measured their maximum absorbance, respectively. After
every cycle, the corresponding degradation rates of
Ag/Fe2O3/ZnO for iodoform and MO were about 92%, 89%,
86%, 85% and 82%, and 75%, 73%, 71%, 70% and 68% (Fig.
8b), respectively. The degradation efficiency of Ag/Fe2O3/ZnO
ternary composite for iodoform and MO solutions dropped
about 10% and 7% after 5 cycles (Fig. 8a), respectively. The
reason may be that Ag/Fe2O3/ZnO ternary composite
participates in the process of degradation, there are some
consumption of Ag/Fe2O3/ZnO after every cycle.
Fig.
6 Time-dependent absorption spectra of iodoform and MO degraded by (a)
Ag/ZnO, (b) Fe2O3/ZnO and (c) Ag/Fe2O3/ZnO.
By considering the peak intensity of MO and iodoform, we
have plotted the corresponding degradation rates of
Fe2O3/ZnO, Ag/ZnO and Ag/Fe2O3/ZnO, as shown in Fig. 7.
Degradation efficiency (y-axis), is defined as (1 − C/C0) × 100%,
and the x-axis is reaction time in units of minute. C0 is the
initial concentration after the equilibrium adsorption, and C is
the remaining concentration of iodoform and MO 18, 19. Under
irradiation of simulated sunlight, the degradation efficiency of
Ag/Fe2O3/ZnO for iodoform and MO were 94% and 80% (curve
1 and 2) after 120 min respectively, much higher than them of
Fe2O3/ZnO (58% and 60%, curve 3 and 4), or Ag/ZnO (56% and
50%, curve 5 and 6). In addition, in the mixture of three
organics, the degradation efficiency of Ag/Fe2O3/ZnO for
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Fig. 8 (a) Cycle times-dependent absorption spectra of iodoform and MO solutions
degraded by Ag/Fe2O3/ZnO ternary composite, and (b) the cycle degradation curves of
Ag/Fe2O3/ZnO for iodoform (curve 1), and for MO (curve 2).
4. Conclusions
In summary, the Ag/Fe2O3/ZnO ternary composite has been
successfully synthesized via chemical deposition and
photochemical deposition in aqueous solution. The
3.5 The proposed mechanism of enhancement of photocatalytical
activity by Ag/Fe2O3/ZnO
Ag/Fe2O3/ZnO ternary composite shows
a much higher
The different component between Ag/Fe2O3/ZnO ternary
composite, Fe2O3/ZnO and Ag/ZnO binary composite may
result in the difference on photocatalytic activities. The
proposed photocatalytic degradation mechanism of iodoform
and MO by Ag/Fe2O3/ZnO is illustrated in Fig. 9. The process
can be described as follows: 1) under illumination, the
electrons of ZnO in the Ag/Fe2O3/ZnO are excited to generate
electron-hole pairs, 2) the electrons in the valence band (VB)
of ZnO are transferred to (CB) conduction band of Fe2O3, 3)
and then they are transferred to CB of Ag. The high separation
rate of electron-hole pairs makes it easier to form O2- active
ion and OH· radicals on the surface of Ag/Fe2O3/ZnO to
degrade iodoform and MO, and to enhance the photo-
photocatalytic performance compared with Fe2O3/ZnO or
Ag/ZnO binary composite. Moreover, the Ag/Fe2O3/ZnO
ternary composite has efficient and selective degradation of
carcinogenic iodoform in the sewage. This provides
a
promising strategy for efficient degradation of halogenated
hydrocarbon.
Acknowledgements
We acknowledge the financial support from the Ministry of
Education of China (IRT1148), the Priority Academic Program
Development of Jiangsu Higher Education Institutions
(YX03001), the Natural Science Foundation of Jiangsu Province
(BK20131376, BY2014015), the Opening Project of State Key
Laboratory of New Ceramic and Fine Processing(KF201310)
and the Synergistic Innovation Center for Organic Electronics
and Information Displays.
degradation activity, the process can be written as 20-25
:
-
O2+e-
O2
(1)
(2)
(3)
(4)
(5)
-
O2 +H+
HO2
H2O2 + O2
OH. + O2+OH-
CO2 + H2O
·
2HO2
H2O2 + O2
OH. + pollutants
·
-
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