Physica E 75 (2016) 66–71

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Physica E
journal homepage: www.elsevier.com/locate/physe

Preparation and photocatalytic properties of magnetically reusable

Fe3O4@ZnO core/shell nanoparticles
Jian Wang a,b, Jinghai Yang c,n, Xiuyan Li c,n, Dandan Wang a,b, Bing Wei c, Hang Song a,
Xuefei Li c, Siwei Fu d
a
Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, Changchun 130033, PR China
b
University of Chinese Academy of Sciences, Beijing 100049, PR China
c
Key Laboratory of Functional Materials Physics and Chemistry of the Ministry of Education, Jilin Normal University, Siping 136000, PR China
d
Changchun Central Hospital, Changchun 130051, PR China

H I G H L I G H T S G R A P H I C A L A B S T R A C T

Fe3O4@ZnO core/shell nano- Magnetically reusable Fe3O4@ZnO core/shell nanoparticles were synthesized by a simple two-step
particles were successful syn- chemical method. Almost no decrease in photocatalytic efficiency was observed even after recycling six
times.
thesized.

The core/shell nanoparticles
show excellent photocatalytic
activity.

Fe3O4 core ensures core/shell
nanoparticles reuse easily in
waste water treatment.

art ic l e i nf o a b s t r a c t

Article history: Fe3O4@ZnO binary nanoparticles were synthesized by a simple two-step chemical method and char-
Received 4 May 2015 acterized using various analytical instruments. TEM result proved the binary nanoparticles have core/
Received in revised form shell structures and average particle size is 60 nm. Photocatalytic investigation of Fe3O4@ZnO core/shell
13 August 2015
nanoparticles was carried out using rhodamine B (RhB) solution under UV light. Fe3O4@ZnO core/shell
Accepted 31 August 2015
nanoparticles showed enhanced photocatalytic performance in comparison with the as prepared ZnO
Available online 3 September 2015
nanoparticles. The enhanced photocatalytic activity for Fe3O4@ZnO might be resulting from the higher
Keywords: concentration of surface oxygen vacancies and the suppressing effect of the Fe3 þ ions on the re-
Fe3O4@ZnO nanoparticles combination of photoinduced electron–hole pairs. Magnetization saturation value (5.96 emu/g) of Fe3O4
Magnetic photocatalysts
@ZnO core/shell nanoparticles is high enough to be magnetically removed by applying a magnetic field.
Photocatalysis
The core/shell photocatalyst can be easily separated by using a commercial magnet and almost no de-
crease in photocatalytic efficiency was observed even after recycling six times.
& 2015 Elsevier B.V. All rights reserved.

1. Introduction

In the last two decades, photocatalysis in the presence of

n
semiconductors caused a wide range of concern because it can be
Corresponding authors. Fax: þ 86 434 3294566.
E-mail addresses: jhyang1@jlnu.edu.cn (J. Yang), lixiuyan@126.com (X. Li).
used in environmental protection [1–4]. Among those

http://dx.doi.org/10.1016/j.physe.2015.08.040
1386-9477/& 2015 Elsevier B.V. All rights reserved.
 J. Wang et al. / Physica E 75 (2016) 66–71 67

semiconductors, ZnO is well-known as an excellent candidate for

photocatalytic reaction owing to its high photocatalytic activity,
environmental compatible feature and relatively low cost [5,6].
Due to photocatalytic process mainly occurs on surface of ZnO
photocatalysts, powder ZnO which have large specific surface area
were utilized in wastewater treatment usually [3,7,8]. However, an
imperative problem to be solved in industry applications of pow-
der ZnO photocatalysts is efficient separation of these fine ZnO
micro/nanoparticles from treated water. Traditional separation
methods always cost too much and may result in secondary pol-
lution caused by photocatalyst loss [9]. Magnetic carriers provide a
very efficient and convenient method for separating and recycling
catalysts by using external magnetic fields [10]. Up to now, most
magnetic photocatalysts have two functional parts at least: a
magnetic component (γ-Fe2O3 or Fe3O4) with the separation
function via an external magnetic field; the second part is the
photocatalytic component with a photocatalytic function, such as
SnO2, ZnO or TiO2 nanoparticles [11–13]. These heterogeneous
catalysts have been proved to be efficient in both separation and
recycle [14]. For instance, Fe3O4/Ag/SnO2 core–shell structured
particles can be removed using an external magnetic field and
their photocatalytic efficiency can still be maintained at 95.74%,
even after eight cycles of use [11]. Thus, develop magnetic pho-
tocatalysts with efficient reusability became a hot research subject
in photocatalytic area [15].
In addition, the introduction of magnetic carriers may result in
the catalytic activity decrease attribute to the decrease of active
ingredient in photocatalyst system [16]. Therefore, semiconductor
shells with high photocatalytic performance were synthesized to
counteract the negative effect of inactive magnetic core [17]. De- Scheme 1. Schematic illustrations of the fabrication of Fe3O4 (a), ZnO (b) and Fe3O4
@ZnO (c).
position of noble metal can enhance photocatalytic activity of
magnetically reusable photocatalyst obviously [16,18,19]. Li et al.
reported RhB in solution can be removed completely by
Fe3O4@SiO2@TiO2@Pt after 20 min UV irradiation while
Fe3O4@SiO2@TiO2 spent 25 min under the same condition [19]. But
expensive cost for noble metal restricted it application in industry.
To decrease the running cost, increase the concentration of surface
defect can enhance activity of ZnO photocatalytic efficiently and
was considered as an economic method [20,21]. Wang et al. re-
ported that the oxygen vacancies can facilitate the photo-
decomposition of 2,4-dichlorophenol under visible light irradia-
tion by ZnO photocatalyst [22]. Enlightened by former studies, it
could be an effective route to obtain high photocatalytic perfor-
mance catalyst by introducing oxygen defects.
Herein, we report our recent research on the synthesis of Fe3O4
@ZnO core/shell nanoparticles. The photocatalytic activities of the
binary composites were evaluated using the degradation of RhB as
a model reaction. It is found that Fe3O4@ZnO core/shell nano-
particles show excellent photocatalytic activity for degrading RhB
in comparison with as prepared ZnO. The enhanced photocatalytic
activity was attributed to the high concentration of oxygen va-
Fig. 1. XRD patterns of synthesized Fe3O4 (a) (the line in below), ZnO (b) (the
cancies and the presence of Fe3 þ ions in the core/shell catalyst.
middle line), and Fe3O4@ZnO (c) (the upper line); the inset image is magnifying
image of the select area in curve (c).

2. Experimental
2.2. Synthesis of Fe3O4 nanoparticles
2.1. Materials and chemicals


Fe3O4 nanoparticles were synthesized through a coprecipita-
Ferric chloride hexahydrate (FeCl3 6H2O), ferrous chloride tion method. The fabrication process was depicted in Scheme 1a.

tetrahydrate (FeCl2 4H2O), sodium hydroxide (NaOH), zinc acetate 
As shown in Scheme 1a, FeCl3 6H2O (6 mmol, 1.622 g) and FeCl2 

dihydrate (Zn(Ac)2 2H2O), ethylalcohol (C2H5OH) were purchased 4H2O (3 mmol, 0.597 g) were dissolved in deionized water
from Sinopharm Chemical Reagent Co. Ltd and used as received. (200 ml). After stirring for 40 min at 55 °C, 100 ml NaOH solution
Deionized water (resistivity 418.0 MΩ cm) was using throughout (0.24 mol L  1) was added to the resulting complex dropwise. Then
the experiment. the reaction mixture was heated at 60 °C for 1 h under mechanical
68 J. Wang et al. / Physica E 75 (2016) 66–71

Fig. 2. SEM images of Fe3O4 (a), ZnO (b) and Fe3O4@ZnO (c); TEM images of Fe3O4 (d), ZnO (e) and Fe3O4@ZnO (f); SEAD image of Fe3O4 (g) and Fe3O4@ZnO (h); HRTEM
images of Fe3O4 (i, j), ZnO (k) and Fe3O4@ZnO (l).

stirring, producing a black suspension. The Fe3O4 were magneti- cooled to room temperature. The obtained precipitation after
cally collected, washed with ethanol and deionized water, and cooling down to room temperature was filtered off, washed three
then dried. times by deionized water and ethanol, and dried at 60 °C for 10 h.

2.3. Synthesis of ZnO nanoparticles

2.4. Synthesis of Fe3O4@ZnO core/shell nanoparticles
As illustrated in Scheme 1b, ZnO nanoparticles were synthe-

sized by a hydrothermal method. Briefly, Zn(Ac2) 2H2O (10 mmol, As shown in Scheme 1c, Fe3O4@ZnO core/shell nanoparticles
2.195 g) and NaOH (20 mmol, 0.8 g ) were dissolved in 30 ml were prepared based on the synthesis of ZnO. For the preparing of
deionized water respectively at first. Then the NaOH solution was Fe3O4@ZnO core/shell nanoparticles, Fe3O4 (2 mmol, 0.463 g) was

added into the Zn(Ac2) 2H2O solution dropwise under stir. The added into the precursor in the process of hydrothermal synthesis
mixture solution was transferred into a Teflon-lined reactor ZnO. The following steps are the same with the procedure for
maintained at 170 °C for 10 h. Subsequently, the system was preparing ZnO nanoparticles described in 2.3.
 J. Wang et al. / Physica E 75 (2016) 66–71 69

Fig. 3. (a) PL spectra of the synthesized ZnO (a-I) and Fe3O4@ZnO (a-II) core/shell
nanoparticles; Gaussian fit results of the 420–750 nm emissions of ZnO nano-
particles (b), Fe3O4@ZnO core/shell nanoparticles (c) with the original curves in
black, the Gaussian fit showing in red, and the green lines showing the fitted peaks.
(For interpretation of the references to color in this figure legend, the reader is
referred to the web version of this article.)

2.5. Characterization

XRD (MAC Science, MXP18, Japan), FESEM (Hitachi S4800), TEM

(JEOL JEM-2100HR, 200 kV), PL (Renishaw inVia micro-PL spec-
trometer, 325 nm, He–Cd laser), VSM (Lake Shore 7407) and UV–
vis spectrophotometer (UV-5800PC, Shanghai Metash Instruments
Fig. 4. (a) Adsorption changes of RhB aqueous in the presence of Fe3O4@ZnO,
Co., Ltd) were used to characterize the crystal structure, (b) Degradation efficiency versus reaction time for ZnO and Fe3O4@ZnO.
morphologies, magnetic and optical properties of the synthesized
samples.

2.6. Photocatalytic degradation of RhB

At the beginning, 60 mg of the synthesized products were

dispersed in 60 mL of the RhB aqueous solution (7 mg L  1) and
the mixed solution was stirred in the dark for 15 min until
reaching the adsorption equilibrium. Then, the mixture solutions
were irradiated under a high-pressure Hg lamp (250 W, wave-
length centered at 365 nm). The concentration reduction of RhB
during photocatalytic experiment was recorded by UV  vis
spectrophotometer.

3. Results and discussion

Scheme 2. A proposed photocatalytic reaction mechanism of the Fe3O4@ZnO.

The crystalline phase and structure of Fe3O4, ZnO, and Fe3O4
@ZnO are studied by XRD analysis. As shown in Fig. 1a, all of the
identified peaks in the XRD pattern can be attributed to magnetite the select area shows two sets of diffraction peaks for Fe3O4@ZnO
Fe3O4, based on the standard data for magnetite (JCPDS no. 19- well indexed to hexagonal wurtzite ZnO and magnetite Fe3O4. No
0629). All the diffraction peaks in the Fig. 1b belong to the wurtzite additional peaks are observed, which confirms that the sample
phase ZnO (JCPDS no. 36-1451), indicating that ZnO have a wurt- only contained nanocrystalline ZnO and Fe3O4. But only base on
zite structure. The blue curve (Fig. 1c) and it magnifying image of the XRD result we can not confirm the combination mode of the
70 J. Wang et al. / Physica E 75 (2016) 66–71

XRD characterization, we can confirm the final obtained binary

compound were Fe3O4@ZnO core/shell nanoparticles.
In order to study the feature of electron–hole pairs on the
surface of photocatalysts, photoluminescence spectra (PL) of as
synthesized ZnO and Fe3O4@ZnO core/shell nanoparticles (λex
¼325 nm) were illustrated in Fig. 3. Both PL spectra in Fig. 3a
consisted of a sharp UV emission peak (λ ¼380 nm) and one broad
peak in the visible region (λ ¼450–700 nm). The sharp UV emis-
sion band generally assigned as a near-band-edge emission band
and the position agrees well with the literature [23,24]. The broad
emission in the visible-light region is associated to ZnO surface
detects, in which oxygen vacancies are the most accepted defects
[25–27]. Changes in the green emission intensity have been as-
sociated to changes in the concentration of the oxygen vacancies
reported in the literature. In our study, by using Gaussian Fitting
the visible emission in spectra can be fitted into green emission
(λ ¼543 nm) and yellow emission (λ ¼588 nm) as shown in the
Fig. 3b and c. The intensity of green emission for Fe3O4@ZnO core/
shell nanoparticles is obviously stronger in comparison with ZnO
nanoparticles. It means more oxygen vacancies existed on the
surface of Fe3O4@ZnO core/shell nanoparticles. Wang et al. re-
ported that the increased surface oxygen vacancies decreased the
surface recombination centers, and improved the charge separa-
tion efficiency [21].
The results of photodegradation RhB are shown in Fig. 4b.
Without any catalyst, only a slow decrease in the concentration of
RhB was detected under UV irradiation. When Fe3O4@ZnO was
added as photocatalyst, 99.3% RhB in aqueous solution could be
eliminated after 60 min of UV irradiation (Fig. 4b-III). ZnO can
eliminate 92.6% RhB in aqueous solution under the same UV ir-
radiation time (Fig. 4b-II).
In many researches on semiconductor photocatalysis, bigger
particle sizes always lead to weaker photocatalytic activity [28].
But in our case Fe3O4@ZnO with bigger particle size shows en-
hanced photocatalytic activity compare with ZnO. That might re-
sult from two reasons. The concentration of surface oxygen va-
cancies was considered as a vital factor to determine the photo-
catalytic performance of ZnO photocatalyst [21,29,30]. Surface
oxygen vacancies can trap photoinduced electrons during the
Fig. 5. Room-temperature magnetic hysteresis loops of Fe3O4 (a) –I, Fe3O4@ZnO (a) photocatalytic process and then prevent the recombination of
–II; the inset image in (a) is the magnetic separation and redispersion process of photogenerated electron–hole pairs. In addition, oxygen species
Fe3O4@ZnO, (b) six cycles of the removal of RhB over Fe3O4@ZnO samples under UV
(such as O2, OH  ) could be adsorbed by surface oxygen vacancies
irradiation.
easily. After reacting with photogenerated carriers, those oxygen
species were transformed into
O−2 and
OH which can accelerate
binary compound. the photocatalysis process.
To investigate the morphology, particle size and crystalline The enhanced photocatalytic activity of Fe3O4@ZnO is also re-
structure of the as synthesized samples, SEM images of Fe3O4, ZnO lated to the presence of Fe3 þ ions in the hybrid nanoparticles.
and Fe3O4@ZnO together with TEM images and the corresponding Ambrus' work proved Fe3 þ ions in Fe3O4 can act as a photo-
HRTEM and SAED are shown in Fig. 2. From SEM and TEM images generated electron-trapping site to prevent the fast recombination
of three samples (Fig. 2a–f), we can observe the average particle of photoinduced charge carriers and prolong their lifetime [31]. As
sizes of Fe3O4, ZnO and Fe3O4@ZnO are 7 nm, 50 nm and 60 nm, shown in Scheme 2, the photoinduced electron in the conduction
respectively. The SAED image (Fig. 2g) and HRTEM image (Fig. 2j) band of ZnO can be captured by Fe3 þ ions in this study. This will
further prove the synthesized Fe3O4 have a magnetite structure. result in the formation of Fe2 þ ions, which are more active in
The HRTEM (Fig. 2k) for ZnO shows clear crystal lattice distance comparison with Fe3 þ ions. Then Fe2 þ ions would react with the
which belong to (100) planes of wurtzite phase ZnO (JCPDS no. 36- O2 dissolved in the reaction solution to generate Fe3 þ ions and
1451). The selected area electron diffraction (SAED) pattern of
O−2 radicals. These
O−2 radicals can destroy the structure of var-
Fe3O4@ZnO core/shell structure is presented in Fig. 2h. The dif- ious organic pollutants, degrading them into non-toxic carbon
fraction dot displayed in the SAED patterns supports the presence dioxide and water [32].
of ZnO in the synthesized core/shell structure. It index to the (100) Easy magnetic separation and recycle are vitally important for
plane of hexagonal ZnO corresponding to JCPDS Card no. 36-1451. the application of photocatalyst in industry. To investigate mag-
The SAED pattern also show the diffraction rings of different netic property of as synthesized samples, magnetic hysteresis
planes of magnetite Fe3O4 (JCPDS 16-0629) confirming the ex- loops of Fe3O4 and Fe3O4@ZnO measured at 300 K are presented in
istence of Fe3O4 in the nanostructures. The HRTEM image (Fig. 2l) Fig. 5a. Both samples have superparamagnetic behavior because
of Fe3O4@ZnO shows a core/shell structure and the crystal lattice almost no remanence or coercivity was observed from the mag-
distances of the core and shell belong to magnetite Fe3O4 and netic hysteresis loops. After coated with ZnO, the magnetization
wurtzite phase ZnO, respectively. Combining with the result of saturation value (MS) of Fe3O4@ZnO (Fig. 5a-II) decreases. The
 J. Wang et al. / Physica E 75 (2016) 66–71 71

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