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Nanoscience and Nanotechnology
All rights reserved Vol. 16, 950–955, 2016
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Electrodeposition of Fe3O4 Thin Film and Its

Application as Anode for Lithium Ion Batteries
Chongchong Zhao1
2 , Ying Ma1 , Cai Shen2
∗ , and Weiqiang Han2
∗
1
School of Materials Science and Engineering, Xiangtan University, Hunan 411105, China
2
Ningbo Institute of Materials Technology and Engineering Chinese Academy of Sciences,
1219 Zhongguan Road, Zhenhai District, Ningbo, Zhejiang, 315201, China

Fe3 O4 films were prepared by electrodeposition under varying preparation conditions (current den-
sity, temperature, and time). The electrodeposited Fe3 O4 were characterized in terms of morphol-
ogy and composition using scanning electron microscopy (SEM) and X-ray diffraction (XRD). The
electrodeposited films were also tested as anode in coin cell systems. Fluoroethylene carbonate
(FEC) electrolyte was found to improve the battery performance due to formation of a better solid
electrolyte interface (SEI). Conducting polymer of polypyrrole (PPY) was coated on the surface of
Fe3 O4 films for the first time with the aim to improve the electric conductivity and to buffer volume
expansion of Fe3 O4 films.
Keywords: Electrodeposition, Fe3 O4 Films, Anode, Lithium Ion Battery.
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Copyright: American Scientific Publishers
1. INTRODUCTION control. Thus, in this paper, we reported a simple elec-
Portable electronic applications such as smart phone, smart trodeposition method for generating thin films of Fe3 O4
watch, and mobile power bank are becoming increas- directly on copper substrates.25–29 Active material (Fe3 O4

ingly popular. As lithium ion battery (LIB) is currently deposited is in good contact with current collector through
the major power source for such devices, there is a huge electrodeposition.30–33 Electrochemical performance of the
market for high capacity and/or high power batteries. 1–3 Fe3 O4 films were tested in two difference electrolytes
Various transition-metal oxides have been studied as elec- (A mixture of ethylene carbonate (EC)/ethyl methyl car-
trode materials for LIB because of their high theoretical bonate (EMC)/dimethyl carbonate (DMC), and a mixture
capacity.4–10 Iron oxide (Fe3 O4 ) has a theoretical capac- of fluoroethylene carbonate (FEC/EMC/DMC). The pur-
ity of 928 mAh/g, which is almost triple of the theo- pose of adding FEC to the electrolytes was to improve the
retical capacity of commercially used graphite carbons quality of the solid-electrolyte interface (SEI) layer and
(372 mAh/g). Fe3 O4 has other advantages including low- to improve the cycling performance of the batteries.34–36
cost and nontoxic. 11–13
It is also a half-metallic mate- Polymer of polypyrrole (PPY) was further introduced onto
rial with improved electrode conductivity as compared to the Fe 3 4 thin film electrodes to improve the electric
O
those with non-conductive materials which require addi- conductivity and to buffer volume expansion of Fe3 O4
37–39
tion of large amount of carbon black to improve the effi- films.
ciency of the cell.13–17 Fe3 O4 thin films have been grown
on various substrates using a variety of deposition tech- 2. EXPERIMENTAL DETAILS
niques such as evaporation, sputtering, and oxidizing.18–24 2.1. Electrochemical Fe3 O4 Films Growth
Although the vacuum-based methods provide good control Fe3 O4 films were deposited directly onto copper electrodes
over film thickness and crystallinity, costly equipments and (14 mm in diameter) by applying a constant cathodic cur-
considerable amounts of energy are required. The aqueous rent (ranging from 5–20 mA) for several deposition dura-
solution-based method such as electrodeposition approach tions (ranging from 60–600 s). A three-electrode setup was
offers advantages such as low cost, flexibility and easy to used for the experiment. A mixed electrolyte solution of
0.05 M Fe2 (SO4 )3 , 1 M NaOH and 0.1 M triethanolamine
∗
Authors to whom correspondence should be addressed. (TEA) was used for the deposition. A mixed electrolyte

950 J. Nanosci. Nanotechnol. 2016, Vol. 16, No. 1 1533-4880/2016/16/950/006 doi:10.1166/jnn.2016.11113

Zhao et al. Electrodeposition of Fe3 O4 Thin Film and Its Application as Anode for Lithium Ion Batteries

solution of 0.05 M Fe2 (SO4 )3 , 1 M NaOH and 0.1 M tri- Table I. Electrodeposition parameters of the Fe3 O4 samples.
ethanolamine (TEA) was used for the deposition. The solu- Electrodeposition Electrodeposition Electrodeposition
tion was prepared by adding Fe2 (SO4
3 to aqueous solution Sample current (mA) temperature ( C) time (s)
containing a mixture of NaOH (1 M) and triethanolamine
1 Fe3 O4 -1 5 95 60
(0.1 M) at room temperature. The solution immediately 2 Fe3 O4 -2 20 95 300
turns into reddish brown precipitate. The solution became 3 Fe3 O4 -3 15 95 300
a pale-green homogeneous color due to the stabilization of 4 Fe3 O4 -4 5 95 300
TEA after 48 hours stirring. The solution was kept in an 5 Fe3 O4 -5 5 75 600
 6 Fe O -6 5 85 600
oil bath at various temperatures (ranging from 75–95 C) 3 4
7 Fe3 O4 -7 5 95 600
in air. Copper disk, carbon paper and platinum wire was
used as working electrode, counter electrode, and reference
electrode, respectively. After deposition, Cu disks were
cleaned with water and ethanol and then dried in air. deposited films. The ideal thin film should have uniform
The synthesis of Fe3 O4 /PPY thin films was performed and dense surface that is composed of nano-sized, well
by a multi-potential step technology. A 60 s of cath- crystallized particles. In this paper, seven Fe3 O4 thin film
ode voltage (1.5 V) was applied to electrodeposite Fe3 O4 samples were prepared for examination. The preparation
film followed by another 60 s of anode voltage (1.5 V) conditions of these samples are summarized in Table I.
to electrodeposite the PPY. This process was repeated For sample 1, 4, and 7, they were deposited as a func-
for 5 times. The electrolyte used for electrodeposition of tion of their electrolysis time for a fixed electrodeposi-
Fe3 O4 /PPY thin films consists of 0.05 M Fe2 (SO4
3 , 1 M tion current and temperature. For sample 2, 3, and 4, they
NaOH, 0.1 M TEA and 0.2 M pyrrole. All electrodepo- were deposited as a function of their electrolysis current
sition experiments were performed using an electrochemi- for a fixed electrodeposition temperature and duration. For
cal workstation (CHI660D, Shanghai Chenhua instrument, sample 5, 6, and 7, they were deposited as a function of
Co. Ltd.). The obtained samples were measured by X-ray deposition temperature for a fixed electrolysis current and
diffraction (XRD, D8 Discover, Broker AXS, Cu radiation, temperature.
 = 1540596 Å) and scanning electron microscopy (SEM, Figure 1 compares the morphology of the Fe3 O4 films
S-4800, Hitachi). deposited at various conditions. It is found that dense
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films were obtained under all condi-
2.2. Electrochemical Properties withCopyright:
Lithium American Scientific
tions tested. Figures 1(a)–(c) show the morphology of the
Publishers
Electrochemical measurements were carried out using films deposited at 95  C for 300 s at currents of 20, 15,
a 2032-type coin cell system. The weights of Fe3 O4 5 mA/sample, respectively. Clearly, the morphology dif-
films before and after deposition were determined using fers significantly at different deposition currents. Specifi-
an analytical balance to the accuracy of 0.01 mg. The cally, at high current of 20 mA/sample (Fig. 1(a)), a very
average loading of Fe3 O4 was ∼0.8 mg/cm.2 2032-type thin layer of porous flake-like thin film formed continu-
coin cells were assembled in an argon-filled glovebox ously and uniformly over the Cu disk. The flakey wall
where oxygen and moisture concentrations are below thickness increased to ∼tens of nanometers as the current
0.1 ppm. Fe3 O4 films were used as working electrode density decreased to 15 mA/sample. Formation of flake
and a lithium wire was used as counter electrode. Cel- structure may be due to the rapid growth of Fe3 O4 which
gard 2400 polypropylene was used as separator. A solu- do not have sufficient time to nucleate and crystallize. Fur-
tion of 1 M lithium hexafluorophosphate (LiPF6 ) dissolved ther reduction of current density to 5 mA/sample resulted
in a mixture of EC/EMC/DMC (1:1:1, volume ratio) in the spinel shape structure which can be observed in
or FEC/EMC/DMC (1:1:1, volume ratio) was used as Figure 1(c).
electrolyte. Charge/discharge measurements were carried Deposition temperature is another critical parameter that
out galvanostatically at various current densities (1C = affects the surface morphology of the deposited films.
928 mAh/g) over a voltage range of 0.01–2.5 V (vs.
Figures 1(d)–(f) show the morphology of the Fe3 O4 films
Li/Li+ ) using a commercial battery test system (LAND
deposited at a constant current of 5 mA/sample for 600 s
model, CT2001A) at room temperature. The cyclic voltam-
at 75, 85, and 95  C, respectively. It was found that flakey
metry (CV) measurement was conducted with electro-
structures similar to the films deposited at high current
chemical workstation (Ametek 1470E).
were formed at low temperature (75  C, Fig. 1(d)). The
structure of the deposited film transformed from flake to
3. RESULTS AND DISCUSSION pebble (Fig. 1(e)), and spinel (Fig. 1(f)) as the deposi-
3.1. Structural and Compositional Characterizations tion temperature increased from 75 to 85, and 95  C,
In electrochemical deposition, deposition parameters such respectively.
as current density, temperature and deposition duration can The effect of the deposition duration on the morphol-
significantly affect the morphology and composition of the ogy is further illustrated in Figures 1(c) and (d). Spinel

J. Nanosci. Nanotechnol. 16, 950–955, 2016 951

Electrodeposition of Fe3 O4 Thin Film and Its Application as Anode for Lithium Ion Batteries Zhao et al.

Figure 1. SEM images of the various Fe3 O4 samples: Fe3 O4 -2 (a); Fe3 O4 -3 (b); Fe3 O4 -4 (c); Fe3 O4 -5 (d); Fe3 O4 -6 (e); Fe3 O4 -7 (f).

shape morphology appears with increased deposition dura- can be attributed to the Cu substrate.32 40 Intensity of
tion from 60 s (sample 1, the surface consists of shape- Fe3 O4 diffraction peaks increased with increasing elec-
less nanoparticles, data no shown) to 300 s (Fig. 1(c)). trodepositon time. For example, sample deposited for 60 s
Faceted particles with salient edges formed when the demonstrated only a weak peak at 31.5 . The strong sharp
deposition duration was increased to 600 s (Fig. 1(f)). peaks of Fe3 O4 obtained after 600 s deposition (with the
Cross-section SEM image of the Fe3 O4 -7 sample illus- (311) reflection being the strongest) suggests good crys-
trates the thickness of the Fe3 O4 films which is approx- tallization of the as-deposited Fe3 O4 under the present
imately 50 m. Atomic force microscope (AFM) study parameters.
confirmed that the Fe3 O 4 -7 sample
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size in the range of 0.5–1 m and a surface roughness
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3.2.
12Electrochemical
Jan 2016 00:14:08Properties of Fe3 O4 Films
100 ± 20 nm. Copyright: American Scientific Publishers
The charge/discharge performances of the Fe3 O4 films
In short, two main factors influenced the film morphol- electrodes with respect to Li were studied at various
ogy (flake, pebble, and spinel) are deposition current den- current rates over a voltage range of 0.01–2.5 V (vs.
sity and temperature. Meanwhile, the deposition duration Li/Li+
. Unexpectedly, the electrochemical performances
affects particle size and thickness of the films. for all samples tested are similar regardless of the mor-
Figure 2 shows the XRD patterns of Fe3 O4 films phology difference of the samples. Figure 3(a) shows the
deposited at a constant current of 5 mA/sample at 95  C charge/discharge profile of the Fe3 O4 -7 sample measured
with different deposition times (samples 1, 4, and 7). with the electrolyte of EC/EMC/DMC at 0.5 C. The ini-
All the main diffraction peaks are in good agreement tial discharge and charge capacities are 1235 mAh/g and
with the diffraction peaks of Fe3 O4 , except for those 604 mAh/g, respectively. Note that the first discharge
diffraction peaks located at ∼43.5, 51 and 74.5 that capacity is larger than the theoretical capacity of Fe3 O4
(ca. 928 mAh/g). The discharge capacity dropped quickly
to a capacity of 574 mAh/g for the second cycle. The
excess capacity of Fe3 O4 and the large irreversible capacity
observed in the first cycle could be explained by forma-
tion of the SEI film due to reactions between the Fe3 O4
particles and electrolyte. A well-defined plateau observed
at the potential of ∼0.75 V is ascribed to the full reduc-
tion of Fe3 O4 into Fe0 /Li2 O mixture (Fig. 3(a)). Due to
the volume expansion and pulverization of Fe3 O4 parti-
cles, a reversible capacity of only 127.6 mAh/g was main-
tained after 30 cycles. The insert in Figure 3(a) shows the
cyclic voltammograms (CVs) for the first cycle between
0.01 and 2.5 V with a scan rate of 0.05 mV/s. A dominant
pair of redox peaks can be clearly observed at ∼0.75 V
and ∼1.6 V during the cathodic and anodic sweep, respec-
Figure 2. XRD patterns of the Fe3 O4 -1, Fe3 O4 -4 and Fe3 O4 -7 samples. tively. The cathodic peak of 0.75 V corresponds to lithium

952 J. Nanosci. Nanotechnol. 16, 950–955, 2016

Zhao et al. Electrodeposition of Fe3 O4 Thin Film and Its Application as Anode for Lithium Ion Batteries

Figure 3. (a) Discharge–charge curves of Fe3 O4 -7 sample with EC/EMC/DMC electrolyte at 0.5 C; insert: the cyclic voltammograms of Fe3 O4 -
7 sample with EC/EMC/DMC electrolyte at a scan rate of 0.05 mV/s for the first cycle; (b) Discharge–charge curves of Fe3 O4 -7 sample with
FEC/EMC/DMC electrolyte at 0.5 C; insert: Cycling performance of Fe3 O4 -7 sample with EC/EMC/DMC electrolyte and FEC/EMC/DMC electrolyte
at 0.5 C.

insertion into Fe3 O4 with the reduction of the Fe0 state, To better understand the role of FEC in the electrolyte,
while the anodic of 1.6 V can be associated with the surface morphology of Fe3 O4 electrodes were examined
reversible oxidation of Fe0 to Fe2+ /Fe3+ , which is consis- after charge/discharge process. Figure 4 compared the
tent with the discharge–charge curves. SEM images of the surface of Fe3 O4 -7 sample after 5
To alleviate the pulverization of Fe3 O4 particles and cycles of charge/discharge under EC and FEC type elec-
improve the cycling performance of Fe3 O4 films, we trolytes. It was found that the morphology of the Fe3 O4
replaced the EC-type electrolyte with FEC-type elec- films changed significantly after cycling under EC elec-
trolyte. Fluoroethylene carbonate (FEC) has attracted trolyte. Cracks with voids were found on the surface
Delivered
many attentions as an ideal additiveby to
Publishing Technology
improve the qual- to:the
of Adelaide
Fe3 O4 Theological Library under EC electrolyte
electrolyte measured
IP: 109.161.197.144 On: Tue, 12 Jan 2016 00:14:08
(Fig. 4(a)), while the surface of Fe3 O4 film measured under
ity of SEI layer and to improve the cycling performance
Copyright: American Scientific Publishers
during the past few years.35 41 42 Figure 3(b) shows the FEC type electrolyte was relatively intact with the surface
discharge–charge curves of Fe3 O4 -7 sample measured with obviously covered with a film (Fig. 4(b)). In short, the
FEC/EMC/DMC electrolyte at 0.5 C. The discharge– FEC-type electrolyte improved the SEI layer and thus min-
charge curves show similar trends as sample measured imizes the damage caused by expansion of Fe3 O4 particles
with EC/EMC/DMC (Fig. 3(a)). However, the cycling (and the pulverization of Fe3 O4 particles).
performance was significantly improved as shown in the
insert in Figure 3(b). After 30 cycles, a reversible capac- 3.3. Structural and Electrochemical Properties of
ity of 371 mAh/g was still maintained. It should be Fe3 O4 /PPY Films
noted that it delivers an initial coulombic efficiency of Although electrodeposition has obvious advantages as
48.9% with EC-type electrolyte, as a comparison, the ini- aforementioned, lack of binding agent and conductive
tial coulombic efficiency increases to 51.9% with FEC- agent degraded the performance of the deposited films.
type electrolyte, and subsequent increase to 89% and To further improve the electrochemical performance of
91.9%, respectively. Overall, the coulombic efficiency with the Fe3 O4 films, conducting polymer of polypyrrole was
FEC-type electrolyte is higher than the EC-type elec- introduced with the aim of improving the electric con-
trolyte, indicating the positive effect of FEC on the SEI ductivity and to buffer the volume expansion of Fe3 O4
layer. films.
Figure 5(a) shows the SEM images of Fe3 O4 /PPY film
obtained by a multi-potential step technology. It was found
that micron balls (few nanometers to micrometers) com-
posed of small Fe3 O4 nanoparticles co-existed on the top
of the Fe3 O4 film due to polymerization effect of PPY.
Figure 5(b) shows the cycling performance of the cell
assembled by Fe3 O4 /PPY electrodes. The capacity reten-
tion is significantly improved after the use of Fe3 O4 /PPY
film. A reversible capacity of 535 mAh/g and 327 mAh/g
Figure 4. SEM images of the Fe3 O4 electrode after 5 cycles in were obtained after 50 cycles and 100 cycles, respectively.
EC/EMC/DMC electrolyte (a) and FEC/EMC/DMC electrolyte (b). In contrast, the pure Fe3 O4 films electrode only shows a

J. Nanosci. Nanotechnol. 16, 950–955, 2016 953

Electrodeposition of Fe3 O4 Thin Film and Its Application as Anode for Lithium Ion Batteries Zhao et al.

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Received: 5 November 2014. Accepted: 12 March 2015.

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Copyright: American Scientific Publishers

J. Nanosci. Nanotechnol. 16, 950–955, 2016 955