Electrochimica Acta 166 (2015) 12–16

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Electrochimica Acta
journal homepage: www.elsevier.com/locate/electacta

Fe2O3-reduced graphene oxide composites synthesized via

microwave-assisted method for sodium ion batteries
Xinjuan Liu 1,a, * , Taiqiang Chen 1,b , Haipeng Chu a , Lengyuan Niu a , Zhuo Sun b ,
Likun Pan b, ** , Chang Q. Sun a
a
Institute of Coordination Bond Metrology and Engineering, College of Materials Science and Engineering, China Jiliang University, Hangzhou 310018, China
b
Engineering Research Center for Nanophotonics & Advanced Instrument, Ministry of Education, Shanghai Key Laboratory of Magnetic Resonance,
Department of Physics, East China Normal University, Shanghai 200062, China

A R T I C L E I N F O A B S T R A C T

Article history: Fe2O3-reduced graphene oxide (RGO) composites were successfully fabricated via a facile microwave-
Received 16 January 2015 assisted reduction of graphite oxide in Fe2O3 precursor solution using a microwave system, and
Received in revised form 10 March 2015 investigated as anode material for sodium ion batteries (SIBs). Their morphologies, structures and
Accepted 11 March 2015
electrochemical performance were characterized by transmission electron microscopy, X-ray diffraction,
Available online 12 March 2015
Raman spectroscopy, cyclic voltammetry and electrochemical impedance spectroscopy, respectively. The
results show that the RGO addition can enhance the electrochemical performance of Fe2O3-RGO
Keywords:
composites. Fe2O3-RGO composite with 30 wt.% RGO exhibits a maximum reversible capacity of
Fe2O3-reduced graphene oxide
microwave assisted synthesis
289 mA h g
1 at a current density of 50 mA g
1 after 50 cycles and excellent rate performance due to the
sodium ion battery synergistic effect between Fe2O3 and RGO. The high capacity, good rate capability and excellent cycle
anode material performance of Fe2O3-RGO composites enable them a potential electrode material for SIBs.
ã 2015 Published by Elsevier Ltd.

1. Introduction high specific capacity and good cycling stability for SIBs remains a
great challenge.
Lithium ion batteries (LIBs) represent a key class of battery Intensive efforts have been made to explore the electrode
architecture that has emerged as a prime candidate for energy materials for SIBs, involving carbon-based materials [14], alloy
storage devices due to their high energy density and long cycle [15], metal oxides and sulfides [16,17]. Among the available
lifetime [1–4]. However, the high cost and possible supply risk of alternative anode materials, Fe2O3 has recently been considered to
lithium resources significantly limits the large scale applications of be a promising electrode material for SIBs due to its excellent
LIBs [5–7]. As a potential alternative, sodium ion batteries (SIBs) chemical stability, high capacity, easy fabrication, low cost and
have recently attracted much attention due to the natural nontoxicity [18–22]. In contrast to layered materials, sodium
abundance, lower cost, and relatively low toxicity of sodium, storage in Fe2O3 is mainly achieved via a reversible conversion
and the similar chemical properties including ionicity, electroneg- reaction, by forming Fe nanoparticles dispersed in Na2O matrix
ativity and electrochemical reactivity between lithium and sodium [23]. However, the reaction is accompanied by considerable
elements [8–13]. Unfortunately, the diameter of sodium ion is volume change upon repeated charge–discharge, which causes
about 55% larger than that of the lithium ion, and only a few host the poor electrical contact, electrode pulverization, and continuous
materials for LIBs are suitable to allow the sodium ion intercalation growth of the solid electrolyte interface (SEI) [24–26]. In addition,
and deintercalation. Therefore, exploring electrode materials with Fe2O3 has a poor electrical conductivity, making the electrochemi-
cal redox reaction difficult. As a result, Fe2O3 suffers from the
relatively low capacity and poor cycling stability, which limits its
commercial potential.
Currently reducing the size and constructing open channels in
* Corresponding author. Tel.: +86 0571 86872475; fax: +86 0571 86872475.
the electrode materials have been suggested to overcome the
** Corresponding author. Tel.: +86 21 62234132; fax: +86 21 62234321.
E-mail addresses: [email protected] (X. Liu), [email protected] (L. Pan). aforementioned problems [18–22,27]. Reversible capacities of
1
The two authors contributed equally to this work. 100–400 mA h g
1 were obtained for the nanostructure Fe2O3.

http://dx.doi.org/10.1016/j.electacta.2015.03.081
0013-4686/ ã 2015 Published by Elsevier Ltd.
 X. Liu et al. / Electrochimica Acta 166 (2015) 12–16 13

However, the poor conductivity and structure pulverization still volume and mean pore diameter were determined by the
exists for pure Fe2O3 anode materials. Another particularly Brunauer–Emmett–Teller (BET) method.
attractive strategy is to design and develop hybrid electrode
materials based on carbon. Recently, various carbonaceous 2.3. Electrochemical Measurement
materials such as carbon nanotubes and carbon fiber have been
reported as the matrix to support the Fe2O3, which not only For electrochemical testing, the as-prepared composites,
enhances its electrical conductivity, but also provides a good Super-P carbon black and polyvinyldifluoride, with weight ratio
accommodation of the large volume change [28,29]. Graphene of 80:10:10, were homogenously mixed in N-methylpyrrolidone
(normally obtained by chemical reduction of graphene oxide (GO) solvent to produce slurry. Then, the resultant slurries were coated
and called as reduced graphene oxide (RGO) with a unique two- on a copper foil using a doctor blading method. Finally, these
dimensional conjugated chemical structure should also be electrodes were dried at 120  C in vacuum for 12 h. Coin-type cells
considered as an ideal matrix in the SIBs because of its large (CR2032) were assembled in a glove box (MB-10-compact,
specific surface area, excellent electrical conductivity and superior MBRAUN) under argon atmosphere with oxygen and water of
chemical stability [30,31]. RGO-based composites have been less than 0.5 ppm, using sodium metal foil as the counter and
demonstrated with the excellent electrochemical performances reference electrode. Whatman glass fiber membrane and 1 M
[32–38]. Therefore, development of composite material based on NaClO4 electrolyte solution dissolved in a mixture of ethylene
Fe2O3 and RGO should be a promising method to enhance the carbonate and propylene carbonate (1:1 w/w) were used as
electrochemical performance of Fe2O3. separator and electrolyte, respectively. Galvanostatic charge–
Herein, a fast strategy was developed to synthesis the discharge cycles were performed using a LAND2001A battery test
Fe2O3-RGO (FG) composites by a microwave-assisted reduction system in the voltage range of 0.005–3 V. Cyclic voltammetry (CV)
of GO in Fe2O3 precursor solution using a microwave system, and was performed using an electrochemical workstation (AUTOLAB
the effect of the RGO amount on the electrochemical properties of PGSTAT302 N) in a voltage range of 0.005–3 V at a scan rate of
FG composite was investigated. Microwave irradiation can 0.2 mV s
1.
facilitate mass production in a short time with little energy cost
[39] and form an intimate contact between Fe2O3 and RGO, which 3. Results and discussion
is crucial for the formation of electronic interaction and
interelectron transfer at the interface [40,41]. Such a micro- The HRTEM images of as-prepared Fe2O3 are shown in Fig. 1(a)
wave-assisted reaction is seldom employed to synthesize FG and (b). Fe2O3 nanoparticles are relatively uniform and dispersive
composites for SIBs. The as-prepared FG composites were used as with diameters of 4–8 nm. The lattice spacing measured for the
anode materials for SIBs and they exhibit improved capacity with crystalline plane is 0.368 nm, corresponding to the (0 1 2) plane of
good cycle stability compared to pure Fe2O3. a-Fe2O3 (JCPDS 33-0664). As shown in Fig. 1(c), when RGO is
introduced, the Fe2O3 nanoparticles are uniformly anchored on
2. Experimental RGO sheets in the FG composite to form a conductive network
structure, which favors fast electronic and ionic transport in
2.1. Synthesis of Fe2O3-RGO composite electrode reactions. The morphologies of FG-10 and FG-50 (not
shown here) are similar as that of FG-30. Fig. 1(d) shows the
GO was synthesized using the method reported in our corresponding selected area electron diffraction pattern (SAED) of
previous works [41,42]. In a typical synthesis, 1.98 g Fe the FG-30. The SAED pattern shows clear diffraction rings, which
(NO3)39H2O, 0.74 g urea and 0.3 g GO were dispersed in 150 ml can be well indexed as a pure a-Fe2O3 phase.
aqueous solution using magnetic stirring and ultrasonic treat- The XRD patterns of Fe2O3 FG-10, FG-30 and FG-50 are shown in
ment to form a homogeneous mixture. Subsequently, 20 ml of the Fig. 2. The peaks in the pure Fe2O3 pattern at 24.1, 33.2 , 35.6 ,
solution was sealed in a 35 ml microwave tube and heated at
150  C with a maximum microwave irradiation power of 100 W
for 10 min using a microwave system (Explorer-48, CEM Co.). The
resultant precipitate was filtered, washed with deionized water,
and finally dried in a vacuum oven at 80  C for 24 h. The as-
synthesized FG composites with 90, 70 and 50 wt.% Fe2O3 by
changing the amount of Fe(NO3)39H2O were labeled as FG-10,
FG-30 and FG-50, respectively. Pure Fe2O3 and RGO were also
synthesized by a direct microwave assisted reaction for compari-
son. As described in our previous work [43], most of the GO can be
reduced to RGO under microwave irradiation and the obtained
RGO has a C/O ratio of 9.12, which is close to the value (10) of
that achieved by the hydrazine reduction method.

2.2. Characterization

The structure and morphology of as-prepared composites

were characterized by high-resolution transmission electron
microscopy (HRTEM, JEOL-2010), X-ray diffraction (XRD, Holland
Panalytical PRO PW3040/60) with Cu-Ka radiation (V = 30 kV,
I = 25 mA, l = 1.5418 Å), and Raman spectra (Horiba Jobin Yvon
T64000) with an excitation wavelength of 532 nm, respectively.
N2 adsorption-desorption isotherms were measured at 77 K with
an ASAP 2020 Accelerated Surface Area and Porosimetry System
(Micromeritics, Norcross, GA) and the specific surface area, pore Fig. 1. HRTEM images of (a-b) Fe2O3 and (c) FG-30; (d) SAED pattern of FG-30.
14 X. Liu et al. / Electrochimica Acta 166 (2015) 12–16

Fig. 4. Nitrogen adsorption-desorption isotherms of Fe2O3 and FG-30.

Fig. 2. XRD patterns of Fe2O3 FG-10, FG-30 and FG-50.

H3 hysteresis loops. The specific surface areas of Fe2O3 and
FG-30 determined form BET method are 47 and 126 m2 g
1,
40.9 , 43.5 , 49.5 , 54.1, 57.6 , 62.4 , 64.0 , 72.3 , and 75.4 are respectively. The results indicate that the introduction of RGO can
indexed to (0 1 2), (1 0 4), (11 0), (11 3), (2 0 2), (0 2 4), (11 6), (1 2 2), increase the specific surface area of Fe2O3, which may enhance the
(2 1 4), (3 0 0), (11 9), and (2 2 0) planes of rhombohedra a-Fe2O3 sodium storage capacity [32,33].
(JPCDS 33-0664), respectively [19]. No other impurity peaks The electrochemical behavior of the FG-30 composite was
appear for pure Fe2O3, indicating the high purity of the as-prepared evaluated by CV analysis as shown in Fig. 5. In the first reduction
sample. The XRD analysis shows that the main diffraction peaks of scan, an irreversible peak is observed at around 0.55 V (vs. Na/Na+),
all the FG composites are similar to those of pure Fe2O3, indicating which originates mainly from the formation of SEI layer [34]. The
that the presence of RGO does not result in the development of new pronounced reduction peak occurs at near 0 V, which is due to the
crystal orientations or changes in preferential orientations of reduction of Fe3+ ! Fe0 [22]. In the anodic scan, two tiny peaks
Fe2O3. No typical diffraction peaks of carbon species are observed appear at 0.68 V and 1.4 V, corresponding to the two step oxidation
in the composite, which may be due to the low amount and Fe0 ! Fe2+ and Fe2+ ! Fe3+ [20,47]. In the following scan cycles, the
relatively low diffraction intensity of RGO, which is similar to those peak at 0.55 V disappears, indicating an irreversible phase
reported in the literatures [41,42,44]. transformation during initial sodium ion insertion and extraction
Fig. 3 shows the Raman spectra of Fe2O3 and FG-30. Three process. Moreover, the CV curves are similar after the first cycle,
characteristic peaks of Fe2O3 at 219 cm
1, 284 cm
1 and 400 cm
1 indicating good repeatability due to the network structure. The CV
correspond to the A1g and Eg modes, respectively, which is in good curves of pure Fe2O3 and RGO were also shown in Fig. S1 (ESIy).
agreement with the previous study [34]. However, the intensity of Compared with pure Fe2O3, the repeatability of FG composites is
these peaks for FG-30 decreases obviously, which may be because better due to the contribution of RGO. The reversible electrochem-
that the Fe2O3 nanoparticles are well embedded inside the RGO ical reaction can be described as: [47]
and thus hardly detectable by Raman spectroscopy [45]. The peaks
at 1354 and 1599 cm
1 in the Raman spectrum of FG-30 are Fe2O3 + 6Na $ 2Fe + 3Na2O (1)
referred as D band corresponding to the breathing mode of k-point Fig. 6 illustrates the first and second charge–discharge curves of
phonons of A1g symmetry and G band assigned to the E2g phonon of the Fe2O3, FG-10, FG-30 and FG-50 electrodes at a current density
sp2 bonds of carbon atoms, respectively. A 2D band with frequency of 50 mA g
1. It can be observed that all the electrodes exhibit a
(2693 cm
1) is also observed in the FG-30, which is an intrinsic large irreversible capacity in the first discharge, which mainly
property of the RGO [43]. FG composites display an increased originates from the decomposition of the electrolyte to form a SEI
intensity ratio of the D peak to G peak (ID/IG) in comparison to that layer on the surface of Fe2O3, and the irreversible intercalation of
of pure GO (Fig. S2 in ESIy), showing a decrease in the average size sodium ions into the crystal lattice [19]. The charge–discharge
of the sp2 domains upon the reduction of GO to RGO [46]. curves of pure Fe2O3 are similar to those of the FG composites, and
Fig. 4 displays the nitrogen adsorption–desorption isotherms of no voltage plateau can be observed for all the electrodes, which is a
Fe2O3 and FG-30. The samples show type IV isotherms with H2 and typical voltage trend of Fe2O3 as reported in the literature [34].

Fig. 3. Raman spectra of Fe2O3 and FG-30. Fig. 5. CV curves of FG-30 electrode.
 X. Liu et al. / Electrochimica Acta 166 (2015) 12–16 15

Fig. 8. Rate performances of FG-10, FG-30 and FG-50 electrodes. The test was
conducted after 50 galvanostatic charge/discharge cycles at a current density of
50 mA g
1.

h g
1, respectively, much higher than that of pure Fe2O3 and RGO.
Although FG-30 electrode delivers a low initial Coulombic
Fig. 6. The first and second charge–discharge curves of Fe2O3, FG-10, FG-30 and FG- efficiency, it increases dramatically upon cycling, and reaches
50 electrodes. over 94% after 5 cycles and 99% after 10 cycles, as shown in Fig. 6,
indicating the excellent reversibility of sodium insertion in the FG
electrodes.
Pure Fe2O3 delivers an initial discharge capacity of 486.8 mA h g
1
The rate performances of the FG-10, FG-30 and FG-50 electrodes
and a reversible capacity of 287.3 mA h g
1, showing a 59% initial
were investigated as illustrated in Fig. 8. Among these electrodes,
Coulombic efficiency. When RGO is introduced, the initial
FG-30 electrode demonstrates best rate performance and delivers
reversible capacity increases to 375.7 mA h g
1 for FG-10 and
reversible capacities of 251.9, 173.8, 89.8, 56.7 and 32.8 mA h g
1 at
reaches a maximum of 389.3 mA h g
1 for FG-30. The relatively
current densities of 0.1, 0.2, 0.5, 1 and 2 A g
1, respectively. The
high reversible capacity is mainly attributed to the network
capacity recovers to 288.4 mA h g
1 when the current density
structure and higher specific surface area. However, when the RGO
returns back to 50 mA g
1. The result reveals that the FG
content is further increased, the initial reversible capacity
composites show a high rate capability and structure stability
decreases to 324.2 mA h g
1 for FG-50, which may be due to the
even at a very high current density.
relatively low capacity of RGO (136.1 mA h g
1). Therefore, the
The enhanced electrochemical performance of FG composites
introduction of RGO with appropriate amount into Fe2O3 can
can be attributed to the synergistic effect between the Fe2O3 and
improve the capacity of Fe2O3.
RGO, which is similar to those reported for LIBs [48,49]. Firstly, the
The cycle performances of the RGO, Fe2O3, FG-10, FG-30 and
conductive network structure in the FG composites can ensure
FG-50 electrodes at a current density of 50 mA g
1 are shown in
efficient and continuous electron transport [34,50]. Secondly, the
Fig. 7. Pure Fe2O3 exhibits a poor cycle performance and the
RGO can act as the buffer layer to accommodate the volume
reversible capacity decreases to about 16 mA h g
1 after 10 cycles.
expansion and prevent pulverization of Fe2O3 during charge and
On the contrary, RGO shows excellent cycle performance and the
discharge process [30,34]. Finally, the large surface area of the FG
reversible capacity almost does not decline after 50 cycles. When
composites can provide a sufficient electrode–electrolyte interface
Fe2O3 and RGO are combined together, the FG composites exhibit
to adsorb sodium ion and facilitate the rapid charge-transfer
improved cycle performance compared to pure Fe2O3. And the
reaction. However, excessive RGO will stick together and signifi-
cycle performance of the FG composites is dependent on the
cantly block the channels for sodium ion diffusion, leading to the
proportion of RGO. With the increase in RGO content, the cycle
decreased electrochemical performance of FG composites [32].
performance enhances. However, with further increase in RGO
content, the cycle performance slightly deteriorates. The optimal
4. Conclusions
value of RGO is 30 wt.%. After 50 cycles, FG-10, FG-30 and
FG-50 electrodes maintain capacities of 72.2, 289 and 192.8 mA
In summary, FG composites were successfully fabricated via a
facile microwave-assisted reduction of GO in Fe2O3 precursor
solution using a microwave system, and investigated as anode
materials for SIBs. The results of electrochemical experiments
demonstrate that the FG composites exhibit excellent cycle
performance with a high capacity and good rate capability due
to the synergistic effect between Fe2O3 and RGO. A maximum
capacity of 289 mA h g
1 at a current density of 50 mA g
1 after
50 cycles is achieved for the FG-30. Even at a high current density
of 1 A g
1, a capacity of 56.7 mA h g
1 is maintained. The high
performance of FG composites provides a potential feasibility for
the anode materials of SIBs.

Acknowledgments

Fig. 7. Cycle performances of RGO, Fe2O3, FG-10, FG-30 and FG-50 electrodes at a Financial support from the National Natural Science Foundation
current density of 50 mA g
1. of China (No. 21401180, 21276087) and the Basic Research Project
16 X. Liu et al. / Electrochimica Acta 166 (2015) 12–16

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