Article

pubs.acs.org/JPCC

Interface Engineering of Perovskite Solar Cell Using a Reduced-

Graphene Scaffold
Mohammad Mahdi Tavakoli,*,† Rouhollah Tavakoli,†,* Soheil Hasanzadeh,‡
and Mohammad Hassan Mirfasih§
†
Department of Materials Science and Engineering, Sharif University of Technology, 14588 Tehran, Iran
‡
Institute of Materials, École Polytechnique Fédérale de Lausanne, Lausanne CH-1015, Switzerland
§
School of Engineering, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo, 113-8656, Japan
*
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ABSTRACT: Interface engineering of solar cell device is a prominent strategy to

improve the device performance. Herein, we synthesize reduced-graphene scaffold
(rGS) by using a new and simple chemical approach. In this regard, we synthesize a
hollow structure of graphene and then fabricate a three-dimensional scaffold of
graphene with a superior surface area using electrophoretic process. We employ this
scaffold as an interface layer between the electron transfer and absorber layers in
perovskite solar cell. The characterization tests and photovoltaic results show that rGS
improves the carrier transportation, yielding a 27% improvement in device performance
as compared to conventional device. Finally, a power conversion efficiency of 17.2% is
achieved for the device based on the graphene scaffold. Besides, rGS amends the
stability and hysteresis effect of the perovskite solar cell.

■ INTRODUCTION
Organic−inorganic perovskite solar cells have generated great
interest worldwide due to the rapid progress of device
performance from 3.8% to 22.1% within only 5 years.1,2 In a
conventional perovskite solar cell, the perovskite film is
sandwiched between electron and hole transfer layers (ETL
and HTL, respectively). Thus, the generated carriers in the
absorber layer need to travel through the ETL and HTL and
their interfaces with perovskite layer. In order to increase the
power conversion efficiency (PCE), it is necessary to precisely
control the carriers along the entire pathway of device.3−6
In this regard, there are many reports on modification of the
carriers transportation in solar cell devices using an interface
layer. For instance, some researchers employed phenyl-C61-
butyric acid methyl ester (PCBM) as an interface layer between
the perovskite and ZnO or TiO2 ETL layers.7−11 They showed
that PCBM improves the carriers transport and decreases
surface recombination and the hysteresis effect, resulting in
higher device performance. Kemp et al.9 deposited a thin ZnO
buffer layer on TiO2 ETL by atomic layer deposition (ALD) to
decrease the interface recombination, yielding a 10% improve-
ment of device efficiency due to the enhancement of the open
circuit voltage (Voc).
Recently, many research groups studied the role of graphene
in the optoelectronic devices. In fact, graphene with a
honeycomb structure, has a high charge carrier mobility up to
106 cm2/V/s, ∼ 98% transmittance throughout the entire
visible light spectrum,12−15 and strong potential for photo-
voltaic applications.16−19 The application of graphene in
perovskite solar cells has recently been the focus of several
studies.20−25 In this regard, some researchers fabricated
nanocomposites of graphene with ZnO and TiO2 nanoparticles
and utilized them as an ETL in the perovskite solar cell,
resulting in a higher current density and device performance.22
Wang et al.23 demonstrated that the combination of graphene
nanoflake and TiO2 nanoparticles could improve the device
performance of perovskite solar cell by up to 15.6%, due to
efficient charge-collection of electrons. Zhu et al.24 employed a
monolayer of graphene quantum dots between perovskite and
TiO2 films and improved the device performance from 8.81 to
10.15%.
In this work, we introduce a simple chemical procedure to
synthesize rGS and utilize it as an interface layer between
perovskite and TiO2 films. In fact, rGS is a three-dimensional
(3D) graphene with porous structure, high surface area, and
good conductivity. In contrast to other works, this is an all-
solution processing route that provides a wide pore structure of
graphene with high loading of perovskite materials for efficient
electron transport. Besides, it has light trapping property that
reduces the reflection. Herein, we utilize the rGS electrode in
the perovskite solar cell architecture. Compared with TiO2/
perovskite and TiO2/2D graphene/perovskite devices, en-
hanced photoinduced current density without Voc drop is
reported for rGS-based device. The results of characterization
Received: June 6, 2016
Revised: August 23, 2016
Published: August 23, 2016

© 2016 American Chemical Society 19531 DOI: 10.1021/acs.jpcc.6b05667

J. Phys. Chem. C 2016, 120, 19531−19536
The Journal of Physical Chemistry C Article

Figure 1. TEM images of the graphene cluster formed after acid leaching. The structure is composed of ultrathin graphene layers with nanoholes.
EDAX analysis of the selected area, marked A in (a), indicates the removal of the zinc oxide from the nanocomposite.

Figure 2. Characterization of the rGS film. (a) Raman spectrum of the rGS film. (b) UV−visible spectra of the ZnO/graphene QDs and rGS films.

tests such as time-resolved photoluminescence (TRPL),

electrochemical impedance spectroscopy (EIS), and external
quantum efficiency (EQE) illustrate that rGS works as a fast
extraction layer for electrons, decreases the charge-transfer
resistance and increases the current density, respectively,
resulting in an efficient perovskite solar cell with a PCE as
high as 17.2%.
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■ RESULTS AND DISCUSSION
An rGS electrode was fabricated as follows:
First, a quasi core−shell structure of ZnO/graphene QDs
was synthesized by a solution process as explained in ref 16.
Briefly, the graphene oxide QDs (Figure S1) were synthesized
by electrolysis16 of a graphite rod and mixed with a solution of
zinc acetate dihydrate in DMF. After 5 h, a quasi core−shell
structure of ZnO/graphene QDs with ∼4 nm average size was
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J. Phys. Chem. C 2016, 120, 19531−19536
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attained, as shown in Figure S2. The TEM images (Figure
S2a,0b) show that the interplanar spacing of ZnO QDs and
graphene nanoshell are 0.26 nm (for (002)) and 0.14 nm,
respectively. Also, energy-dispersive X-ray spectroscopy
(EDAX) analysis (Figure S2c) and X-ray diffraction pattern
(Figure S2d) support the formation of a quasi core/shell
structure of zinc oxide/graphene QD.12,17
Second, a diluted hydrochloric acid solution (5 wt %) was
used to remove the ZnO core from the core−shell structure.
Thus, the ZnO/graphene QDs were dispersed in the acidic
solution with aggressive stirring for 2 h at 50 °C. This treatment
leached out the ZnO core, and the warped graphene shells were
partially unfolded and formed a cluster. Figure 1a shows a
cluster of reduced graphene oxide after removing the ZnO core.
As seen, this structure is porous with many holes, which is
consisted of several ultrathin graphene layers. In fact, the
structure may be the result of agglomeration of graphene shells
after dissolving the ZnO core. As shown in Figure 1b, the
interatomic spacing of the shells is 0.14 nm, which is matched
with graphene. In order to confirm the composition of the
graphene cluster, EDAX analysis of the selected area (marked A
in Figure 1a) is performed. As can be seen in Figure 1c, the
composition of this cluster is pure carbon with negligible
amount of oxygen. In addition, X-ray photoelectron spectros-
copy (XPS) confirms the removal of the ZnO core (Figure S3).
Figure 2 shows the Raman and UV−visible spectra of the
graphene clusters. As can be seen in Figure 2a, there are three
peaks at 1346.4 (D band), 1578.5 (G band), and 2668 cm−1
(2D band), which are related to the existence of defects and
disorders in the graphitic sheets after ZnO removal, the
vibration of sp2-bonded carbon in the graphene lattice, and a
shell with a few layers of graphene, respectively. The high ID/IG
ratio shows the enhancement of the disorder level in the
graphene cluster after removing the ZnO core. A blue shift in
the absorption peak of the graphene clusters (from 375 to 268
nm) confirms the removal of the ZnO core (Figure 2b).
Third, an rGS electrode is deposited on TiO2-coated FTO
glass using electrophoretic deposition (EPD) from a solution of
graphene clusters. Figures 3a and S4 show the top-view and
cross-sectional SEM images of rGS, indicating a porous
structure with large surface area. Figure 3b shows the
transmittance spectra of the rGS layer compared to the two-
dimensional (2D) graphene layer (see more details in the
Supporting Information (SI)) and TiO2-coated FTO glass. The
results indicate that the graphene layers (2D or 3D structure)
decrease the transmittance. Interestingly, the rGS demonstrates
a higher transmittance than the 2D graphene layer due to the
light trapping property.
Figure 3c shows the top-view and cross-sectional SEM
images of CH3NH3PbI3 perovskite film on the rGS layer
fabricated by a two-step solution process explained in the SI,
indicating a highly crystalline perovskite film. Meanwhile, the
effect of interface layer on perovskite film and its crystal size is
studied by using high-resolution SEM. As shown in Figure S5,
the morphology of perovskite film is influenced by its interface
layer. The results indicate that the average grain size of
perovskite film on top of graphitic interface layer is larger than
TiO2-based film. Moreover, the rGS-based film has the largest
grain size, indicating a high quality perovskite film. The XRD
pattern of perovskite film on top of the rGS is in good
agreement with the literature and shows a highly crystalline
structure of perovskite film with a cubic crystal structure
(Figure 3d).8
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Article
Figure 3. (a) Top-view SEM image of the rGS structure, (b)
transmittance spectra of the rGS, 2D graphene, and TiO2 films, (c)
top-view SEM image of perovskite film on rGS, and (d) XRD pattern
of perovskite film.
Figure 4a shows a cross-sectional SEM image of the
perovskite solar cell on the rGS electrode. In the device
architecture, the FTO glass is coated by a thin film of TiO2
blocking layer. The 2D and 3D reduced graphene oxide is
deposited on the TiO2-coated FTO glass by an EPD method.
Thereafter, the perovskite film (∼300 nm) is formed on top of
the electrode using a two-step solution process, followed by an
annealing process at 100 °C for 45 min. To complete the device
structure, the HTL, that is, 2,2′,7,7′-tetrakis(N,N-di-p-methox-
yphenylamine)-9,9′-spirobifluorene (Spiro-OMeTAD) is spin-
coated on the perovskite film, and finally, 100 nm thick gold is
thermally evaporated as top electrode. Figure 4b shows the
current density−voltage (J−V) of perovskite devices based on
different types of ETLs under simulated AM 1.5G solar
irradiation in the air. The results demonstrate that the device
on the rGS has a PCE as high as 17.2%, with a short current
density (Jsc) of 22.8 mA/cm2, a Voc of 1.05 V, and a fill factor
(FF) of 72%. This indicates 13% and 27% improvement
compared with the devices on 2D graphene layer and
conventional devices, respectively. The figures of merit for all
the devices are summarized in Table 1. As can be seen, the Voc
of the devices on different electrodes remains almost
unchanged. In fact, the role of the graphene layer at the
interface is the enhancement of the Jsc and FF of solar cell
devices. In addition, the external quantum efficiency (EQE) of
the devices is in good agreement with the results of the J−V
measurement, as shown in Figure 4c. On the other hand, the
rGS increases the EQE of the perovskite device, resulting in a
higher Jsc. Furthermore, the device based on the rGS illustrates
a higher EQE than the device on 2D graphene layer due to its
light trapping property inside the rGS (Figure 3b) and the
larger surface area in contact with perovskite film.
Moreover, the rGS has another significant role in the
perovskite solar cell, and that is, reducing the hysteresis effect.
Figure 4d shows the J−V measurements of the devices on the
rGS, 2D graphene, and TiO2 using forward and reverse scan
directions. Note that the result of the J−V measurements for
device on rGS electrode are slightly different compared with
counterpart devices, as indicated in Table S1.
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Figure 4. Characteristics of perovskite solar cells based on different interfacial layers such as an rGS, which acts as a fast electron extraction layer. (a)
Cross-sectional SEM image of the device on the rGS (inset image is the high magnification of cross-sectional area which is shown by red box), (b) J−
V curves under 1.5 AMG indicate the performance of the devices, (c) EQE spectra, (d) J−V measurement of devices in forward and reverse scan
directions, and (e) stability of the devices in an ambient environment (∼65% humidity) after encapsulation using UV-cured epoxy.

Table 1. Figure of Merits for the Prepared Perovskite Solar Cells Based on the rGS, 2D Graphene, and TiO2a
device based on Voc (v) Jsc (mA/cm2) FF (%) avg PCE (%) maximum PCE (%) Rs (Ω) Rct (Ω)
TiO2 1.04 ± 0.05 19.1 ± 1.1 68 ± 3 11.7 ± 1.8 13.5 27.8 247.1
2D graphene 1.05 ± 0.02 20.7 ± 0.8 70 ± 1 13.6 ± 1.7 15.3 21.2 108.4
rGS 1.05 ± 0.03 22.8 ± 0.9 72 ± 2 16.2 ± 1 17.2 17.6 92.7
a
All values are the average values of 12 devices.

Moreover, the rGS electrode improves the stability of the
perovskite device, as shown in Figure 4e. In this case, all devices
were sealed by using UV-cured epoxy and measured over one
month in the ambient environment (∼65% humidity). The
results indicate that the PCE of device on the rGS drops only
20% of the initial value after 30 days, which is more stable than
TiO2-based device with 65% loss.
To further study the role of rGS electrode on device
performance and support our findings, TRPL and EIS
measurements are employed, as illustrated in Figure 5a and b,
respectively. The result of the TRPL measurements shows that
perovskite films on the rGS and 2D graphene layer have shorter
lifetime than TiO2-based one, as shown in Figure 5a. The fitting
parameters of the corresponding PL decay curves are shown in
Table S2. As seen, the device on the rGS has the shortest
lifetime compared with counterpart devices (17 and 98% lower
than devices on 2D graphene and TiO2, respectively).19 The
results of steady-state photoluminescence are consistent with
the TRPL results, as demonstrated in Figure S6. In fact, the
19534
quenching effect in the presence of graphene is primarily caused
by the static quenching and charge transfer reactions.22 In
addition to dynamic quenching, static quenching occurs when
the donor and acceptor materials are in the ground state,
resulting in an improvement of efficient charge carrier
extraction. Moreover, the carriers transfer is also faster than
the charge recombination process using the rGS electrode, as
evidenced by the TRPL measurement.
Besides, the role of rGS electrode is investigated by
electrochemical impedance spectroscopy (EIS) analysis. Figure
5b shows the results of EIS tests for perovskite devices on the
rGS, 2D graphene layer, and TiO2. As seen, the Nyquist curves
of the devices have plotted in dark condition (Z′ vs −Z″),
where Z′ and Z″ are the real and imaginary parts of the cell
impedance, respectively. As illustrated in Figure 5b and Table 1,
the charge-transfer resistance of the devices based on the
graphene electrode is lower than TiO2, one due to the smaller
radius of the semicircle. Here, the rGS device shows the lowest
charge-transfer resistance. The values of ohmic resistance and
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Figure 5. Device characterizations. (a) Time-resolved PL spectra of perovskite film based on different interfacial films, (b) EIS spectra of the
perovskite solar cells on different interfacial layers, (c) Band diagram of perovskite solar cells on rGS, and (d) the rGS work function was measured
using an ultraviolet photoelectron spectrum (UPS).
charge-transfer resistance for rGS device are calculated using
the inset model in Figure 5b, which are 17.6 and 92.7 Ohm,
respectively. The calculated values from the EIS curves are
shown in Table 1. The results confirm that the rGS device has
fast electron transport properties and lower carrier recombina-
tion compared with its counterpart, as witnessed by the higher
Jsc. The results of the TRPL and EIS tests for the rGS-based
device demonstrate the faster and more efficient electron
transfer than radiative and nonradiative decay of photo-
excitations, resulting in the lower charge recombination
process.26−30
Beside ultraviolet photoelectron spectroscopy (UPS) was
employed to study the band alignment diagram of perovskite
device on the rGS, as shown in Figure 5c. The Fermi level of
the rGS is calculated from the curve in Figure 5d. He I (21.2
eV) is utilized as photon source for UPS measurement. It is
worth pointing out that the band level of the rGS matches with
the perovskite film very well and, as a result, the electrons are
transferred from the perovskite film into the TiO2 ETL easily
through the rGS electrode. In the rGS-based device, the
photogenerated electrons flow from rGS to TiO2 ETL due to
the lower energy level of TiO2 as compared to rGS.
In fact, our findings indicate that the rGS electrode is
matched with perovskite film well due to its suitable work
function. As mentioned in the literature,23,24 there are many
defects and recombination sites on the surface of TiO2 film,
resulting in lower current density in the perovskite solar cell.
Thus, the presence of an interface layer such as rGS can help to
improve the efficiency of the device by passivation of the
dangling bonds on the surface of TiO2 ETL. Owning to the
properties of rGS such as excellent charge transfer, high
conductivity, fast extraction of electrons, larger surface area, and
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Article
light trapping properties, we establish a highly efficient
perovskite solar cell based on rGS electrode.
■
CONCLUSIONS
In summary, we present a new all solution processing approach
to fabricate a porous structure of graphene (rGS) on FTO
glass. This method is based on the synthesis of a quasi core/
shell structure of ZnO/graphene QDs and dissolution of ZnO
core using an acidic solution, following by EPD of graphene
clusters. We employed rGS as an interface layer for fabrication
of perovskite solar cell. Compared with conventional devices,
rGS-based perovskite solar cell shows better charge transfer and
lower carrier recombination, resulting in higher Jsc (30%) and
PCE. Furthermore, the lower work function of the rGS than the
conduction band of perovskite film may facilitate the
transferring of the photoinduced electrons to the rGS with
better conductivity. Our findings suggest that an rGS electrode
could serve as an excellent interface layer in a perovskite solar
cell, which improves the carriers transfer and the PCE of the
device. Finally, a PCE of 17.2% with low hysteresis is achieved
based on rGS electrode.
■
*
ASSOCIATED CONTENT
S Supporting Information
The Supporting Information is available free of charge on the
ACS Publications website at DOI: 10.1021/acs.jpcc.6b05667.
Experimental methods, the characterization and analysis
tests of graphene oxide quantum dots and ZnO/
graphene QDs, photoluminescence spectra of perovskite
devices on different substrates, AFM analysis of GO
DOI: 10.1021/acs.jpcc.6b05667
J. Phys. Chem. C 2016, 120, 19531−19536
The Journal of Physical Chemistry C
sheets, and the details of J−V measurement results
(PDF).
■
AUTHOR INFORMATION
Corresponding Authors
*E-mail: mmtavakoli@ust.hk. Tel.: (852) 54948635. Fax: +98
(21) 6600 5717.
*E-mail: rtavakoli@sharif.ir.
Notes
The authors declare no competing financial interest.
■
ACKNOWLEDGMENTS
We thank funding support from the Grant Program of Sharif
University of Technology (No. G930305) and Elite National
Institute.
■
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