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Temperature-assisted rapid nucleation: a facile

Cite this: J. Mater. Chem. A, 2017, 5,
method to optimize the film morphology for
20327 perovskite solar cells†
Ying-Ke Ren,a Xi-Hong Ding,a Ya-Han Wu,a Jun Zhu, *b Tasawar Hayat,c
Ahmed Alsaedi,c Ya-Feng Xu,d Zhao-Qian Li,d Shang-Feng Yang e
and Song-Yuan Dai *acd

Received 19th July 2017
Accepted 21st August 2017
DOI: 10.1039/c7ta06334b
rsc.li/materials-a
The nucleation stage has an important influence on the lead halide perovskite film morphology, and
therefore the solar cell performance. Here, we introduce a facile temperature-assisted rapid nucleation
(TRN) method to improve the film crystallization process and the film morphology. By employing low
temperature anti-solvents (diethyl ether, chlorobenzene and toluene), we stimulate homogeneous
nuclei growth, resulting in a highly dense perovskite thin layer. The TRN method prepared
(FAPbI3)0.85(MAPbBr3)0.15 devices exhibit a power conversion efficiency up to 19.2% and maintain over
85% of the original efficiency after 40 days of storage at room temperature under a relative humidity of
10–40%.

pin-hole free perovskite lms.11 Therefore, various strategies

Introduction have been developed to induce the nucleation process, such as
In a short span of a few years, tremendous development has gas-assisted methods,12 solution printing,13 additive
been made in the perovskite solar cell (PSC) eld due to the approaches, illumination and solvent quenching,15–17 etc.
14

strong light absorption, high carrier mobility and long carrier-
diffusion length of lead halide perovskite materials.1–4
Following the rst report on a 3.8% efficient perovskite solar
cell in 2009,5 the record power conversion efficiency (PCE) of
PSCs has dramatically raised to over 22%.6 Fabricating high-
quality perovskite layers, which are mainly characterized by
high surface coverage, low surface roughness and well-crystal-
lized grains, is believed to be crucial for achieving high PCE.2
Generally, nucleation and growth govern the lm
morphology.7,8 Previous reports have uncovered that a few
nuclei on the surface generate a large crystal grain size with the
disadvantage that pin-holes are le between the grains.9,10
Rapid nucleation and retarded growth are critical in obtaining
a
Beijing Key Laboratory of Novel Thin-Film Solar Cells, North China Electric Power
University, Beijing, 102206, China. E-mail: sydai@ipp.ac.cn
b
Key Lab of Special Display Technology, Ministry of Education, National Engineering
Lab of Special Display Technology, State Key Lab of Advanced Display Technology,
Academy of Opto-Electronic Technology, Hefei University of Technology, Hefei,
230009, China. E-mail: zhujzhu@gmail.com
c
NAAM Research Group, Department of Mathematics, Faculty of Science, King
Abdulaziz University, Jeddah 21589, Saudi Arabia
d
Key Laboratory of Photovoltaic and Energy Conservation Materials, Institute of
Applied Technology, Hefei Institutes of Physical Science, Chinese Academy of
Sciences, Hefei, 230031, China
e
University of Science and Technology of China, Hefei 230026, China
† Electronic supplementary information (ESI) available. See
10.1039/c7ta06334b
Among these methods, anti-solvent dripping would accelerate
solvent extraction from the solution, which leads to fast
nucleation thereby promoting high surface coverage perovskite
lms.9 However, it remains a signicant challenge to nely tune
the nucleation speed during the lm crystallization process.
The processing temperature has been suggested to play an
important role in the nucleation and growth of perovskite
lms.10,18,19 Li and co-workers found that the MAPbI3 (MA ¼
CH3NH3) crystallinity increases with the increase of MAI solu-
tion temperature during the two-step solution process.19 Choi
and co-workers derived a theoretical model equation from the
Gibbs free energy and pointed out that the MAPbI3 nuclei
number decreases with the increase of two-step reaction
temperature.18 A larger grain size with the increase of reaction
temperature was also experimentally observed. Snaith and co-
workers employed heated airow during the one-step spin
coating procedure and stimulated uniformly distributed nuclei
growth as observed by microscope imaging. A pin-hole free
perovskite layer was obtained and an average PCE of 17.6% was
achieved for the resulting planar device.10
In this context, we developed a temperature-assisted rapid
nucleation (TRN) technique for crystal engineering of perov-
skite layers. By systematically investigating the inuence of anti-
solvent temperature on the crystallization process of perovskite
lms, it can be found that the nuclei number increases with
DOI:
decreasing temperature of anti-solvents. We use cold anti-
solvents for the rst time during the one-step spin coating

This journal is © The Royal Society of Chemistry 2017 J. Mater. Chem. A, 2017, 5, 20327–20333 | 20327

Journal of Materials Chemistry A
procedure, which enables swi nucleation through the whole
surface of the substrate. Inducing rapid nucleation which could
produce smooth dense perovskite lms enabled the fabrication
of PSCs with a PCE over 19% regardless of the hysteresis effect,
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while attaining a higher degree of reproducibility.
Results and discussion
The schematic diagram of the TRN method for preparing highly
dense perovskite lms is illustrated in Fig. 1a. First, the
perovskite precursor solution was spin-coated on a mesoporous
TiO2 layer at 4000 rmp. The lms were then quickly washed with
diethyl ether (DE) at different temperatures before the surface
turned turbid. For simplicity, the corresponding perovskite
lms washed with DE at different temperatures were named as
D-30, D-20, D-10 and D-0, respectively. These numbers repre-
sent the temperatures of DE. Finally, the perovskite layers were
obtained by heating at 105  C for 10 min.
The X-ray patterns of the perovskite lms were measured to
reveal the inuence of the DE temperature on their crystallinity.
Fig. 1b shows the evolution of the X-ray patterns of perovskite
layers with decreasing the DE temperature. All of the prepared
lms displayed the typical diffraction peaks of the MAPbI3
perovskite tetragonal phase, including two notable character-
istic peaks at 14.2 and 28.4 which correspond to (110) and
Fig. 1 (a) Schematic illustration of the TRN process for fabricating perovskite films. (b) The XRD patterns and (c) UV-Vis measurements of
perovskite films washed with DE at different temperatures. (d) The steady-state photoluminescence curves for the perovskite films upon
excitation at 450 nm.
20328 | J. Mater. Chem. A, 2017, 5, 20327–20333
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(220), respectively.20 Furthermore, with the DE temperature
decreasing from 30 to 0  C, the intensity of peaks was signi-
cantly enhanced, suggesting increased crystallinity.21 The high
crystallinity of the MAPbI3 lm remarkably affects its optical
properties. The perovskite lms from dripping 0  C DE showed
stronger absorption (Fig. 1c), which was attributed to the
increased crystallinity and possibly reduced reection.22 Fig. 1d
shows the PL spectra of glass/MAPbI3 (D-30, D-20, D-10 and D-0)
lms. All samples were prepared on bare glasses to avoid the
effects of charge injection among the active layer and FTO.
From Fig. 1d, it is clearly shown that the PL intensities increase
with decreasing the DE temperature, implying that the high
quality lms have fewer surface defects and enhanced crystal-
linity.23 In addition, a uorescence peak centered at about 775
nm was also observed, which was in good agreement with the
literature.23
Fig. 2 shows the top-view SEM images of the perovskite lms
from dripping DE at different temperatures. As can be seen in
Fig. 2e, perovskite lms with large particle sizes are formed at
30  C. Although absorber lms with large particles are bene-
cial for charge transport, the cell performance indeed decreased
due to the existence of open grain boundaries.22 The large gaps
between particle boundaries might result in charge leakage
between the electron and the hole transporting materials.24
With the DE temperature decreasing from 30  C to 20  C, the
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Paper
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Fig. 2 Top-view scanning electron microscopy (SEM) images of perovskite films from dripping DE at different temperatures, (a and e) D-30, (b
and f) D-20, (c and g) D-10 and (d and h) D-0.
large gaps reduced and became pin holes between the grains
(Fig. 2b), indicating an enhanced nucleation. When the
temperature was decreased to 10 and 0  C, we could observe
a densely connected perovskite (Fig. 2c, d, g and h). The grains
in the top area of the perovskite lm were almost linked
together, which will favor valid charge transport in the cell.
To understand the effect of DE temperature on the perov-
skite lm crystallization process, we captured in situ optical
micrographs during thermal annealing. Fig. 3a–r show the
images of the perovskite lms (D-30, D-20 and D-0) at different
stages of crystallization. Here, we assigned the perovskite crys-
tallites in the optical image to the dark colored region
embedded within the blue precursor phase. The sample from
dripping DE at 30  C (D-30) shows a small number of nuclei on
the surface, leading to poor coverage of the substrate (Fig. 3a–f).9,10
Nevertheless, when the temperature was decreased to 20  C, the
D-20 shows uniformly distributed nuclei with full coverage. These
results conrmed that the DE temperature inuenced the stage of
nucleation, which determines the nal morphology of perovskite
layers. Fig. 3s shows the difference of nucleation stages of
perovskite lms from dripping warm and cold DE. The role of cold
DE is to facilitate homogeneous nucleation and thereby result in
full coverage of the substrate. In the case of warm DE (30  C),
cluster aggregation is increased due to the slow nucleation stage
with different crystallization processes, leading to large gaps
between perovskite grains. When the cold DE (0  C) was applied to
the perovskite lm, just aer spin coating (that is, t0), some
distinctive rod-like brown interconnected crystals appeared
within the blue background, as shown in Fig. 3m. However, we do
not observe such brown domains in the lm from dripping DE at
20 and 30  C (Fig. 3a and g). These images clearly suggest that the
low temperature DE (0  C) would induce faster nucleation, leading
to a dense perovskite lm. As the annealing progresses, these rod-
like brown colored crystals are gradually dissolved (that is, from t0
to t0 + 25 s). Meanwhile, small spherical brown colored crystals
appeared over the entire substrate and became much larger
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Journal of Materials Chemistry A
(Fig. 3o–q). We ascribe this phenomenon to the Ostwald ripening
process.22,25
Based on the above investigations, the underlying mecha-
nism of the formation process of perovskite grains in the TRN
method is proposed. Fig. 3t shows that the PbI2, MAI and DMSO
were rst dissolved in DMF and combined into a precursor
solution. A transparent and light yellow intermediate phase was
obtained during the spin coating, while the anti-solvent (cold
DE at 0  C) accelerated the perovskite nucleation from the
precursor solution. Then, the nuclei dissolved and aggregated
into spherical crystals under annealing conditions. With
increasing reaction time, much larger spherical perovskite
crystals were formed owing to the Ostwald ripening process.25
Finally, perovskite layers with high crystallinity were obtained
via re-crystallization. In a perovskite solar cell, the quality of
perovskite layers can directly inuence the photovoltaic
performance. Therefore, we studied the photovoltaic perfor-
mance of PSCs from dripping DE at different temperatures
(Fig. S1†), and the corresponding detailed device parameters are
given in Table S1.† From Fig. S1 and Table S1,† we can see that
the as-obtained D-0 based PSCs exhibit higher short-circuit
current density and open-circuit voltage than other PSCs (D-30,
D-20 and D-10). The PCE of the PSC from dripping cold DE
(0  C) was promoted to 17.2%, in accordance with the densely
connected perovskite as conrmed by SEM in Fig. 2.
To further investigate the universality of the TRN method, we
also fabricated perovskite lms using two other anti-solvents,
chlorobenzene (CBZ) and toluene. In addition, mixed cation
lead iodide perovskites are widely used as perovskite materials
for preparing high-performance solar cells.26 Hence, the top-
view SEM images of (FAPbI3)0.85(MAPbBr3)0.15 perovskite lms
from dripping CBZ at different temperatures were obtained.
The corresponding perovskite lms were named as C-40, C-20
and C-0, respectively, and the numbers represent the CBZ
temperatures. As shown in Fig. 4, similar to DE, the higher
temperature CBZ (Fig. 4d) leads to open grain boundaries and
the cold CBZ (Fig. 4e and f) leads to densely connected
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Fig. 3 (a–r) Optical microscopy images recorded during thermal annealing of the perovskite films from dripping DE at different temperatures. (s)
Illustration of the nucleation and growth of the grains treated with warm and cold DE. (t) Schematic reaction process from the precursor to
perovskite grains via cooling crystallization and Ostwald ripening processes.

perovskite grains. Compared with C-20, the surface topography
of C-0 appears to be slightly more at. A similar result is
observed for perovskite lms from dripping toluene at different
temperatures (Fig. S2†). In addition, the statistical particle size
for perovskite lms based on DE and CBZ is shown in Fig. S3.†
When the temperature of anti-solvents was decreased to 0  C,
the perovskite particle size based on D-0 (or C-0) became slightly
smaller than others. Although these closely packed small
perovskite grains inevitably increased the grain boundary
number, the grain boundaries in the top area of the perovskite
lm may have a negligible or even benecial impact on the
performance of perovskite solar cells.27 These results demon-
strated that the TRN method is a universal method for
preparing high quality perovskite lms.
As mentioned above, cold anti-solvents are benecial to the
formation of dense perovskite thin lms. Thus, we studied the
photovoltaic performance of PSCs prepared by tuning the CBZ
temperature. Fig. 5a shows the typical photovoltaic character-
istics of the PSCs, and the corresponding detailed device
parameters are listed in Table 1. The PSC from dripping low
temperature CBZ (0  C) exhibited higher short-circuit current
density (JSC) due to the enhanced absorption and charge
transportation.28 The open-circuit voltage (VOC) showed
a signicant increase with the decrease of CBZ temperature,
indicating reduced defect-induced recombination in the
device.11 The photovoltaic performance of the perovskite solar
cell from dripping cold CBZ (0  C) was dramatically promoted to
19.2%, in accordance with the densely connected perovskite as
conrmed by SEM in Fig. 4. The internal photo-current effi-
ciency spectrum (IPCE) was measured to understand the
changes in JSC. As shown in Fig. 5b, the IPCE of the cell (C-0) had
a very broad plateau over 80% between 350 and 750 nm, further
verifying its excellent photoelectric conversion characteristics.
The integrated current density was calculated to be 20.3, 21.6,

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Fig. 4 Top-view SEM images of perovskite films washed with chlorobenzene at different temperatures, (a and d) C-40, (b and e) C-20, (c and f)
C-0.

Fig. 5 (a) The current density–voltage curves of PSCs from dripping CBZ at different temperatures. (b) Internal photo-to-current efficiency
measurements and the corresponding integral current density for the devices. (c) Current density–voltage curves of PSCs with different scanning
directions. (d) The transient absorption decay at 760 nm for the perovskite films upon excitation at 500 nm. (e) The electrochemical impedance
spectra (EIS) of the PSCs. (f) Statistical PCE for the PSCs (from 30 samples for each condition).

Table 1 Parameters of current density–voltage curves of PSCs and and 22.7 mA cm2 for the corresponding solar cells, respec-
the transient absorption decay lifetimes of perovskite films tively. These results were quite consistent with the JSC obtained
from the photovoltaic curves (Fig. 5a). In addition, as can be
JSC Average
PSCs (mA cm2) VOC (V) FF (%) PCE (%) PCE (%) s (ns) seen from Fig. 5c, the hysteresis effect of the J–V curves is
negligible. The statistic PCE of the 30 solar cells along with the
C-40 20.3 0.95 71.8 13.8 12.7 12.8 Gaussian tting is also displayed in Fig. 5f. For the low
C-20 21.6 1.06 75.3 17.2 15.8 20.1 temperature CBZ (0  C) processed solar cells, it had an
C-0 22.7 1.08 78.2 19.2 18.4 44.7
impressive average PCE of 18.4% over 30 devices, which
demonstrated its outstanding reproducibility.

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Journal of Materials Chemistry A Paper

dense perovskite lms for highly efficient perovskite conversion

can be easily regulated by the TRN process. The champion
(FAPbI3)0.85(MAPbBr3)0.15 device based on the TRN method
exhibited a PCE of 19.2% under AM 1.5 G solar illumination of
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100 mW cm2. The reproducible fabrication process by

controlling the temperature of anti-solvents is expected to
facilitate industrial scalable manufacturing of PSCs in future.

Conflicts of interest
There are no conicts to declare.

Fig. 6 Stability of perovskite solar cells for 40 days. All devices were
stored in the dark at room temperature (10–25  C) and humidity of 10–
Acknowledgements
40%. The insets are the corresponding contact angle measurements of This work was supported by the National Basic Research
C-30, C-20 and C-0.
Program of China under Grant No. 2016YFA0202400 and
2015CB932200, the National Natural Science Foundation of
China under Grant No. 21403247, the Distinguished Youth
It is generally believed that the photovoltaic performance is
Foundation of Anhui Province (1708085J09), and the Major/
inuenced by the carrier lifetime.29 Thus, the transient
Innovative Program of Development Foundation of Hefei
absorption decay was measured to research charge carrier
Center for Physical Science and Technology (2016FXZY003).
recombination behavior in perovskite layers. The results could
be tted to single exponential decays and detailed t charge
lifetimes are listed in Table 1. Clearly, the carrier lifetime tted References
from C-0 (44.7 ns) shows the longest decay lifetime, indicating
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