Ceramics International 43 (2017) 33143318

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

NiTiO3/Ag3PO4 composites with improved photocatalytic activity under

visible-light irradiation

MARK

Gao-yu Zhao , Yu Zhang, Lin Jiang, Hong-mei Zhang

The Coal Chemical Engineering 2011 Collaborative Innovation Center of Guizhou province, Key Laboratory of Applied Chemistry of Guizhou province, School
of Chemical Engineering, Guizhou University of Engineering Science, Bijie 551700, PR China

A R T I C L E I N F O

A BS T RAC T

Keywords:
Photocatalysis
Photodegradation
Ag3PO4
NiTiO3
Composite

A series of NiTiO3/Ag3PO4 composites were prepared by a simple ion-exchange deposition method. The
composition and morphology of the samples were determined by XRD, EDS and SEM. UVvis DRS was used to
characterize their optical absorption properties. The loading of NiTiO3 could promote the ecient separation of
photoinduced electron-hole pairs and enhance the charge carrier transport to improve the photocatalytic
activity. The APO-5 composite exhibited the best photocatalytic activity for the degradation of methyl violet
(MV). Kinetics studies indicated that the APO-5 composite showed an apparent rate constant of 0.115 min1,
which was 2.61 times that of pure Ag3PO4.

1. Introduction
In recent years, photocatalysis has become one of the most popular
research issues due to its great potential to solve energy shortages and
environmental pollution [14], ever since the photocatalytic properties
of TiO2 were discovered by Fujishima [5]. However, because of its large
band gap (3.2 eV for anatase), TiO2 can respond to only UV light,
resulting in the ineective use of solar energy. Accordingly, it is
imperative to develop ecient visible-light photocatalysts. Based on
this, as is currently required, many visible-light photocatalysts have
emerged, such as BiVO4[6], g-C3N4[7,8], BiOI [9], Ag3VO4[10],
Ag3PO4[11] and graphene-based materials [12,13].
Owing to its outstanding photocatalytic activity in water splitting
and waste-water clean-up under visible-light irradiation, Ag3PO4 has
captured substantial attention in the past few years [11,1416]. Thus
far, there are two main strategies to improve the stability or photocatalytic activity of Ag3PO4: one is to fabricate Ag3PO4 nanostructures
with dierent morphologies [11,15,1719], and the other is to
assemble composites by coupling Ag3PO4 with other semiconductors
such as Ag3PO4/CeO2[20], Fe3O4-Ag3PO4[21], Ag3PO4-bentonite [22],
Ag3PO4-graphene [23], Ag3PO4/TiO2[24,25], Ag3PO4/SnO2[26],
Ag3PO4/BiOI [27], Ag3PO4/BiOBr [28], NiFe2O4/Ag3PO4[29],
Ag3PO4/BiPO4[30], AgX/Ag3PO4 (X = Cl, Br, I) [31,32], and CQDs/
Ag3PO4[33]. Using these strategies, the photocatalytic activities of
these materials has been greatly improved. To theoretically provide a
plausible explanation for recent experimental results, rst-principles
density functional theory and the LDA+U formalism have been used to

explore the origin of the photocatalytic activation of Ag3PO4[34].

Nickel titanate (NiTiO3) has been widely explored for its suitable
band gap (approximately 2.18 eV) and unique photoresponse in the
visible-light region for photocatalysis. Porous NiTiO3 nanorods have
been fabricated by a facile ethylene glycol-mediated route [35]. The
material exhibited excellent photocatalytic performance in the degradation of the organic toxic pollutant nitrobenzene (NB) under visiblelight irradiation, proving its potential applications in the elds of
environmental protection. Fu and coworkers prepared heterogeneous
CdS/NiTiO3 by means of growing CdS nanoparticles on the surface of
NiTiO3 nanorods through a chemical bath deposition method [36]. The
composite exhibited improved visible-light photocatalytic activity and
stability in the photocatalytic reduction of Cr(VI) compared with single
CdS nanoparticles and NiTiO3 nanorods. Yuan and coworkers fabricated a novel g-C3N4/NiTiO3 composite by a one-step calcination
method [37]. The photocatalytic activity of the as-prepared composites
was measured by the degradation of NB under visible-light irradiation.
A NiTiO3/g-C3N4 hybrid photocatalysts prepared by a dierent method
also exhibited enhanced activity in photocatalytic water splitting [38].
Zhang et al. synthesized a heterojunction nanobre of -Fe2O3/NiTiO3
by a two-step method involving a calcining process [39]. The -Fe2O3/
NiTiO3 heterojunction nanobres exhibited enhanced performance in
the photodegradation of the organic dye Rhodamine B (RhB).
To the best of our knowledge, there has been no research on
NiTiO3/Ag3PO4 composites. Herein, we successfully prepared a series
of NiTiO3/Ag3PO4 composites by a simple ion-exchange deposition
method, which showed excellent capability for MV degradation under

Corresponding author.
E-mail address: gansonzhao@163.com (G.-y. Zhao).

http://dx.doi.org/10.1016/j.ceramint.2016.11.169
Received 22 September 2016; Received in revised form 22 November 2016; Accepted 23 November 2016
Available online 24 November 2016
0272-8842/ 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Ceramics International 43 (2017) 33143318

G.-y. Zhao et al.

visible-light irradiation. The composites were characterized by X-ray

diraction (XRD), eld-emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS) and UVvisible diuse
reectance spectroscopy (UVvis DRS). The results of the photocatalytic activity tests suggested that APO-5 possessed the best activity for
MV degradation.
2. Experimental
2.1. Materials and sample preparation
All reagents were of analytical purity and were used without further
purication. Nickel acetate (Ni(CH3COO)2)4H2O), tetra-n-butyl titanate (Ti(OC4H9)4), ethylene glycol, silver nitrate (AgNO3), polyvinyl
pyrrolidone (PVP), and potassium phosphate monobasic (KH2PO4)
were purchased from Shanghai Aladdin Industrial Co., Ltd. NiTiO3 was
synthesized according to the literature [35].

Fig. 1. XRD patterns of NiTiO3, Ag3PO4 and NiTiO3/Ag3PO4 composites.

and a 300 W Xe lamp was used as the visible-light source. Before

irradiation, the suspension was stirred for 40 min to reach an adsorptiondesorption equilibrium. During irradiation, approximately 4 mL
of the suspension was collected every 10 min and ltrated by lter
membrane to remove the suspended photocatalyst particles. The
concentration of MV dye was measured by UVvis spectrophotometry
at room temperature.

2.1.1. Preparation of NiTiO3

In a typical synthesis, 4.96g nickel acetate (Ni(CH3COO)2)4H2O)
and 3.4 mL tetra-n-butyl titanate (Ti(OC4H9)4) were dissolved in
120 mL ethylene glycol, and the solution was stirred at room temperature for approximately 10 min. A light blue precipitate appeared and
increased gradually. The mixture was stirred for 1 h to make sure the
reaction was complete. The light blue precipitate was obtained and
puried three times by centrifugation with ethanol and dried under
vacuum at 60 C for 2 h. Finally, the light blue precipitate was calcined
at 600 C for 2 h in air to obtain NiTiO3 nanorods.

3. Results and discussion

3.1. Characterization of NiTiO3/Ag3PO4 samples

2.1.2. Preparation of NiTiO3/Ag3PO4

The NiTiO3/Ag3PO4 composite was prepared by a simple ionexchange deposition method. Typically, AgNO3 (0.510g, 3 mmol) was
dissolved in 20 mL distilled water. Ammonia aqueous solution (1.0 M)
was added dropwise to obtain a transparent solution (silver ammonia
solution), and 0.500g PVP was dissolved in this solution. Then, 0.005g
NiTiO3 was dispersed into the solution. After sonication for 5 min, a
10 mL aqueous solution of KH2PO4 (0.10 M) was added dropwise to
the above dispersion under stirring, and the resulting mixture was then
stirred for another 30 min. The precipitates were separated by centrifugation, washed 3 times with distilled water and 1 time with
ethanol, and then dried under vacuum at 60 C for 2 h. This sample
was considered APO-5. The composites with dierent amounts of
NiTiO3 were prepared by adding the corresponding amounts of NiTiO3
(2 mg, 10 mg, or 20 mg) into the silver ammonia solution and were
considered APO-2, APO-10 and APO-20, respectively.
Ag3PO4 was prepared by a similar method without adding NiTiO3,
considered APO.

The structural identity and composition of the as-prepared pure

NiTiO3, pure Ag3PO4 and NiTiO3/Ag3PO4 composites were investigated by examining their X-ray diraction (XRD) patterns (Fig. 1). The
patterns of a-e are highly consistent with that of Ag3PO4 (JCPDS No.
06-0505) [33]. No apparent peaks corresponding to NiTiO3 in the
patterns of the composites were observed (Fig. 1b-e), and the most
likely reason was that the amount of NiTiO3 in the composites is too
low. The peaks of NiTiO3 matched well with those of the standard
structure of ilmenite NiTiO3 (JCPDS No. 33-0960) [35] (Fig. 1f). No
other characteristic peaks were observed in the XRD patterns.
To conrm the existence of NiTiO3 in the NiTiO3/Ag3PO4 composites, the sample APO-5 was selected and detected by EDS analysis
(Fig. 2d). As seen in the gure, peaks attributed to Ni, Ti, Ag, O and P
were observed, which were indicative of the NiTiO3 and Ag3PO4
components present in the composite. In addition, the quantitative
results are listed in Table 1.
Fig. 2 shows the SEM images of Ag3PO4, NiTiO3 and an NiTiO3/
Ag3PO4 composite. As seen in Fig. 2a, pure Ag3PO4 consists of
agglomerates composed of sphere-like particles, and their average
diameter is approximately 200 nm. In addition, pure NiTiO3 is rodlike, and the length of the NiTiO3 nanorods is approximately 12 m
(Fig. 2c). In the composite, Ag3PO4 grew on the surface of the NiTiO3
nanorods. This further conrmed the existence of NiTiO3 in the
composite.

2.2. Characterization
The crystal structures of the samples were determined by X-ray
powder polycrystalline diraction (Rigaku Ultima IV) using graphite
monochromatized Cu-K radiation (=1.54 ). The XRD patterns were
scanned in the range of 580 (2) at a scanning rate of 5 min1. The
morphology of the samples was investigated by eld-emission scanning
electron microscopy (FE-SEM), which was equipped with an energydispersive X-ray spectroscope (EDS) operated at an acceleration
voltage of 5 kV. The diuse reectance spectra (DRS) were obtained
using a UVvis spectrophotometer (Shimadzu UV-2700, Japan) in the
range of 200800 nm with BaSO4 as the reectance standard material.

3.2. Optical absorption properties

The UVvis DRS spectra of NiTiO3, the NiTiO3/Ag3PO4 composites
and Ag3PO4 are shown in Fig. 3a. As shown in the gure, Ag3PO4
showed strong absorption in the visible-light region. Over the range of
490800 nm, the loading of NiTiO3 enhanced the optical absorption
intensity to a certain extent, while over the range of 200490 nm, the
eect of NiTiO3 on the absorption intensity was relatively small. The
APO-5 composite exhibited the strongest absorption intensity among
these composites. Compared with pure Ag3PO4, the band edge position
of APO-5 exhibited a small red shift, and their g are 590 nm and

2.3. Photocatalytic experiments

The photocatalytic performances of six as-prepared samples were
evaluated by the photodegradation of MV. Typically, 0.200 g powder of
photocatalyst was added into the solution of MV (100 mL, 10 mg L1),
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G.-y. Zhao et al.

Fig. 2. SEM images of Ag3PO4 (a), an NiTiO3/Ag3PO4 composite (b) and NiTiO3 (c). In addition, EDS patterns of APO-5 (d).

where , h, and A are the absorption coecient, Plank's constant, the

light frequency, and a constant, respectively. The band gap energies for
the samples were determined from plots of (h)1/2 versus h, as
shown in Fig. 3b. The band gap energies of NiTiO3 and Ag3PO4 were
estimated to be 2.28 eV and 2.17 eV. The Eg of NiTiO3 is close to that of
previously results (2.18 eV) [39]. In addition, the Eg of Ag3PO4
(2.17 eV) is low compared to the standard value (2.44 eV), which
might be ascribed to the dierent preparation methods. Moreover, the
Eg of the APO-5 composite is 2.10 eV, which is lower than that of pure
Ag3PO4, and this can be attributed to the formation of the NiTiO3/
Ag3PO4 heterojunction, as the heterojunction has a lower energy gap
and could improve the light absorption ability [41].

Table 1
The EDS quantitative results of APO-5.
Element
Line

Net Counts

Int.
Cps/
nA

Weight %

Weight
% Error

Atom %

Atom
%
Error

OK
PK
Ti K
Ni L
Ag L
Total

1893
3011
177
489
15980

3.786
6.022
0.354
0.978
31.960

13.11
5.22
1.36
2.72
77.59
100.00

45.98
9.46
1.59
2.60
40.37
100.00

0.40
0.12
0.25
0.35
1.52

1.41
0.21
0.30
0.33
0.79

571 nm, respectively.

The band gap energy (Eg) of the samples was estimated by the
following formula based on the UVvis DRS results [40]:

3.3. Photocatalytic activity

The photocatalytic performances of NiTiO3/Ag3PO4 composites
were evaluated in MV aqueous solution (10 mg L1) under visible-light
irradiation at room temperature. Before irradiation, the mixture of the

h = A(h Eg)2

Fig. 3. UVvis DRS spectra of NiTiO3, Ag3PO4 and the NiTiO3/Ag3PO4 composites (a) and the band gap energy (Eg) of NiTiO3, Ag3PO4 and the APO-5 composite (b).

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Fig. 4. (a) Photodegradation curve of MV under visible-light irradiation in the presence of the composite samples. (b) Kinetics rate constants for the photodegradation of MV by the
NiTiO3/Ag3PO4 composites.

of Ag3PO4, where the holes can serve as active sites for MV photodegradation. The essence of the mechanism is that the formation of
heterojunctions promoted the separation of photoinduced electronhole pairs, as well as charge carrier transfer, and improved the
photocatalytic activity of the photocatalysts. Fig. 5.
4. Conclusion
This article provided a facile method for preparing NiTiO3/Ag3PO4
composites with improved photocatalytic activity. The experimental
results showed that the APO-5 composite possessed excellent photocatalytic activity for MV degradation under visible-light irradiation,
which could be ascribed to the ecient separation of photoinduced
electron-hole pairs and enhanced charge carrier transfer. In conclusion, the fabrication of semiconductor composites is indeed an eective
way to improve the photocatalytic activity of photocatalysts, which will
gain increasing attention in the eld of photocatalysis.

Fig. 5. The proposed photodegradation mechanism of MV by the NiTiO3/Ag3PO4

composite.

MV aqueous solution and the photocatalyst was stirred in the dark for
40 min to reach adsorption-desorption equilibration. Fig. 4a shows the
MV photodegradation over Ag3PO4 and NiTiO3/Ag3PO4 composites. As
shown in Fig. 4a, pure Ag3PO4 exhibited a removal rate of 89.3% after
40 min of visible-light irradiation (before irradiation, the decrease in
concentration is because of adsorption). The APO-5 composite showed
the best photocatalytic activity among the samples, as more than 99.5%
of the MV molecules were removed within 40 min.
In accordance with the previous studies [42], it was suggested that
the photodegradation of dye obeyed pseudo-rst-order kinetics. The
pseudo-rst-order kinetics for the degradation of MV were calculated
as follows:

Acknowledgements
This work was nancially supported by the Science and Technology
Fund of Guizhou Province ([2015]2055), the Science and Technology
Cooperative Planning of Guizhou Province (LH[2016]7055, LH[2016]
7056, LH[2016]7058), and the High-Level Talents Fund of Guizhou
University of Engineering Science (G2015002).
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