Materials Science in Semiconductor Processing 150 (2022) 106940

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Materials Science in Semiconductor Processing

journal homepage: www.elsevier.com/locate/mssp

Improvement of green antisolvent-isopropanol and additive-thiourea on

carbon based CsPbIBr2 perovskite solar cells
Qingchen He a, Haiming Zhang a, *, Siqi Han a, b, Yuwen Xing a, Yujie Li a, Xianjing Zhang a,
Rufeng Wang a
a
School of Physical Science and Technology, Tiangong University, Tianjin, 300387, China
b
Intelligent Manufacturing College, Tianjin Sino-German University of Applied Sciences, Tianjin, 300350, China

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

Keywords: In recent years, all-inorganic perovskite cells (PSCs) have been widely studied by researchers because of their
CsPbIBr2 excellent thermal and optical stability. Among them, the CsPbIBr2 PSCs with carbon electrode have attracted
Isopropanol extensive attention because of its excellent stability, low preparation difficulty, easy commercialization and low
Green antisolvent
cost. However, the crystal quality of CsPbIBr2 film is poor. There are a large number of pinholes and surface
Thiourea
defects (Pb2+ exposure), which will lead to internal short circuit and a large number of nonradiative recombi­
Lewis base
Passivation interface nation, thus affecting the photoelectric conversion efficiency (PCE). Although these problems can be improved
All-inorganic perovskite solar cells by antisolvent engineering, the traditional antisolvent chlorobenzene (CB) and toluene (TL) are highly toxic and
harmful to the environment. In this paper, isopropanol (IPA) is used as a green antisolvent to improve the quality
of CsPbIBr2 films, and S2− with strong reducibility and passivation defects are successfully introduced into the
CsPbIBr2 film surface by further adding thiourea as Lewis base to IPA (IPA-S). After the CsPbIBr2 films were
treatment by IPA-S antisolvent, we successfully obtained high-quality CsPbIBr2 films with large grain size and no
pinholes. Moreover, through XPS, PL, EIS and other tests, it is found that the S2− introduced by IPA-S can
combine with the exposed Pb2+ on the CsPbIBr2 surface to passivate the defects, it is beneficial to reduce the non-
radiative recombination and improve the transport capacity of carriers. Finally, the results of this paper prove
that that the champion PCE of carbon based CsPbIBr2 PSCs treated with IPA-S antisolvent was 6.79%, which was
nearly 30% higher than the original carbon based CsPbIBr2 PSCs. In addition, due to the strong reducibility of
S2− , the carbon based CsPbIBr2 PSCs treated with isopropanol antisolvent added with thiourea can continue to
work in air with 40% relative humidity, and the efficiency can remain 85% within 10 days. In order to improve
the performance and stability of the all-inorganic PSCs, this paper provides a non-toxic, environmentally friendly
and effective scheme.

1. Introduction
As we all known, the perovskite solar cells (PSCs) have been widely
studied and concerned because of their high absorbance, high photo­
electric conversion efficiency (PCE) in theory, excellent photoelectric
characteristics, simple preparation process and low cost for easy
commercialization [1–4]. In the ten years since the first appearance of
the PSCs, the PCE of PSCs (25.7%) have far exceeded that of traditional
silicon solar cells, which shows that the PSCs have a very broad prospect
[5].
Compared with organic-inorganic PSCs, the all-inorganic PSCs
(CsPbIBr2 PSCs) have excellent heat resistance and photochemical
stability, and have the advantages of simple preparation process, low
energy consumption, low raw material cost and easy commercial pro­
duction [6,7]. In this paper, in order to further reduce the preparation
cost and simplify the preparation process, we use carbon electrode as
hole transport layer and electrode to replace expensive organic hole
transport layer (HTL) (such as Spiro-OMeTAD) and noble metal elec­
trodes (such as Ag, Au) [8–12].
However, due to the material properties of the perovskite, the
perovskite films prepared by solution method were polycrystalline films,
and the perovskite films with high density defects will inevitably be
produced [13–16]. Therefore, in order to reduce the defects of the
perovskite films, researchers have put forward many research schemes

* Corresponding author.
E-mail address: zhmtjwl@163.com (H. Zhang).

https://doi.org/10.1016/j.mssp.2022.106940
Received 12 January 2022; Received in revised form 23 June 2022; Accepted 29 June 2022
Available online 8 July 2022
1369-8001/© 2022 Published by Elsevier Ltd.
Q. He et al.
for preparing the high-quality perovskite films in the past. Such as,
antisolvent assisted crystallization engineering [17,18], gas blow assis­
ted crystallization [19], one or two-step sequential spin-coating depo­
sition [20], vacuum flash assisted crystallization [21,22],
solution-crystal secondary growth [23], and chemical vapor assisted
solution process [24]. Among these methods, antisolvent engineering
have become the mainstream method to prepare high crystalline quality
perovskite films by adjusting nucleation and crystal growth due to the
advantages of many kinds of antisolvents available, simple operation, no
additional equipment and low cost. According to the research of Alex­
ander W. Stewart, isopropanol, as a green non-toxic anti solvent of
perovskite, can effectively improve the crystallinity and an extended
lifespan. This paper draws on some results of Alexander W. Stewart’s
research [25].
Antisolvent can promote the formation of perovskite crystal seeds in
perovskite precursor solution, which provides supersaturation power for
the preparation of high crystalline quality perovskite films [26]. Because
dimethyl sulfoxide (DMSO) and dimethylformamide (DMF) have high
polarity as perovskite solvents, and chlorobenzene (CB) and toluene (TL)
are low polar compounds with benzene ring structure, which are the
preferred materials for traditional antisolvent engineering. However, CB
and TL are highly toxic and carcinogenic, which are extremely harmful
to human body and natural environment [27]. Moreover, their high
volatility point and low boiling will cause a large amount of CB or TL
vapor in the operating environment at relatively warm temperature,
which will lead to poor morphology, many defects and poor reproduc­
ibility of the prepared perovskite films [28,29]. Furthermore, in the
thermal annealing stage, the residual CB and TL in the operating envi­
ronment and on the perovskite film may interrupt the secondary growth
of perovskite crystals [30,31].
Except for antisolvent engineering, previous researchers add addi­
tional additives to the perovskite precursor solution to control the
growth of perovskite and or passivate perovskite defects to prepare more
perfect perovskite films, which is called additive engineering. Many
additives have been proved to be helpful to prepare high-quality
perovskite films. The research of additives is mostly based on coordi­
nation or ionic bond, so additives have various effective functional
groups, such as –CN, Cl− , S2− , NH3+, –OH, –COOH and –C– – O which
have been introduced to interact with uncoordinated ions of perovskite
film [32–38].
For example, Qi et al. The results show that NH3+on ammonium
iodide (NH4I) can be used as Lewis base to passivate uncoordinated
Pb2+and control the nucleation and crystal growth of perovskite by
forming Pb–NH4 bond [38]. In addition, Wang et al. introduced sulfur
ions by adding cesium xanthate (CsXth) to perovskite [1], and the sulfur
ions filled in the lattice gap of perovskite to form a combination, which
stabilized the ɑ-phase of perovskite and improved its moisture resistance
while improving the PCE of the PSCs.
In this paper, we used isopropanol (IPA) and thiourea to fabrication
CsPbIBr2 perovskite film. As a low toxic green antisolvent, IPA can
rapidly precipitate the CsPbIBr2 crystal seeds from CsPbIBr2 precursor
solution, providing supersaturation power for the preparation of the
CsPbIBr2 films with high crystal quality. Thiourea, as an additive, can
provide S2− (Lewis base) after low temperature treatment to effectively
passivate the undercoordinated Pb2+ ions, leading to passivation of
defect states.
As a Lewis base that can provide additional electrons, S2− can also
form coordination compounds with Pb2+ in CsPbIBr2 precursor solution,
so as to delay the crystallization speed of CsPbIBr2 crystals, reduce the
enthalpy required for CsPbIBr2 crystallization and increase the crystal
size, so as to prepare high-quality CsPbIBr2 films. The photovoltaic
performance of the CsPbIBr2 PSCs treated by IPA and thiourea (IPA-S
CsPbIBr2 PSCs) shows that the champion PCE is 6.79%, which is 30%
higher than the PCE for the original CsPbIBr2 PSCs. Moreover, the IPA-S
CsPbIBr2 PSCs have better oxidation resistance and moisture resistance
than the original CsPbIBr2 PSCs. In order to improve the performance
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Materials Science in Semiconductor Processing 150 (2022) 106940
and stability of the all-inorganic PSCs, this paper provides a non-toxic,
environmentally friendly and effective scheme.
2. Experimental section
2.1. Materials. Isopropanol (C3H8O, 99%, anhydrous), Thiourea
(CH4N2S, 99%, anhydrous) and dimethyl sulfoxide (DMSO, anhydrous)
from Sigma-Aldrich; lead bromide (PbBr2, 99.99%, anhydrous) and ce­
sium iodide (CsI, 99.99%, anhydrous) from Xi’a Polymer Light Tech­
nology Corp.; conductive carbon slurry from Mater Win New Materials
Company, China, Shanghai; Tin oxide (SnO2),15% in colloidal disper­
sion from Alfa (China) Aesar Company;
2.1. Device fabrication
FTO glass (2 cm × 2 cm) needs to be cleaned by ultrasonic cleaning
machine and washed with detergent and ultrapure water for one time for
20 min, deionized water for 3 times for 15 min, ethanol for one time for
15 min and isopropanol for one time for 30 min respectively. After
cleaning, in order to further remove the organic residues on the surface
of FTO glass, it is necessary to clean with a plasma cleaning machine for
15 min.
The Tin dioxide (SnO2) precursor solution was diluted to 2.67 wt%
with ultrapure water and stirred 15 min. The 80 μl SnO2 precursor so­
lution (2.67 wt%) was dropped onto FTO glass, then spun it at 800 rpm
for 5 s and 2600 rpm for 20 s, and then calcined at 153 ◦ C for 35 min to
obtain SnO2 film. In order to make the perovskite precursor solution
easier to spin on the SnO2 film, the SnO2 films need to be treated by
plasma for 15 min.
The CsPbIBr2 precursor solution was made by dissolving PbBr2 (660
mg) and CsI (468 mg) in DMSO (1500 μl) and stirring overnight at 60◦ C.
Mix thiourea and isopropanol (IPA) to form isopropanol-thiourea (IPA-
S) solution with the concentration of 7 mmol/L. Both CsPbIBr2 precursor
solution and IPA-S solution need to be filtered by needle filter (PTFE
type, 200 nm aperture) before use. The perovskite layers were deposited
by spun an 80 μL mixed perovskite solution in a two-step procedure: i)
800 rpm for 10 s, and subsequently ii) 3000 rpm for 40 s. During the
second step, 200 μL different antisolvents of IPA and IPA-S were dropped
at the last 10th s, respectively. The wet perovskite film needs to be
placed for 5–7 min, then annealed the wet film at 260◦ C for 10 min.
Finally, the conductive carbon slurry was evenly scraped and coated on
the perovskite film with a knife and tape, and then annealed at 120◦ C on
the heating table for 15 min. All the operations are carried out in the
glove box.
2.2. Measurement and characterization
The surface morphology of the CsPbIBr2 films were measured by
Gemini 300 type scanning electron microscope (SEM). The chemical
states of the CsPbIBr2 surface were measured by the energy dispersive X-
ray spectrometers (EDS) in the (SEM) and the X-ray photoelectron
spectra (XPS) with helium gas admitted employing the HeI (21.22 eV)
emission line by EscaLab Xi+. The UV–visible absorption spectrums
(UV–vis) of the CsPbIBr2 films were measured by PerkinElmer UV
WinLab Lambda35. The photoluminescence spectroscopy (PL) of the
CsPbIBr2 films were measured by F-7000 FL Spectrophotometer. The X-
ray diffraction patterns (XRD) of the CsPbIBr2 films were measured by
Rigaku D/MAX 2500 with Cu and K radiation. The electrochemical
impedance spectroscopies (EIS) of the CsPbIBr2 PSCs were measured by
CHI760E type electrochemical workstation under dark conditions. The
current–voltage curves (J-V curves) of the CsPbIBr2 PSCs were measured
by Enlitech SS-F7-3A under AM 1.5G (100 mW/cm2) illumination. The
external quantum efficiency spectra (EQE) of the CsPbIBr2 PSCs were
measured by Enlitech QE-R with the wavelength range of 300–700 nm.
Q. He et al.
3. Discussion
The SEM images of the original CsPbIBr2 film, the CsPbIBr2 film
treated with isopropanol (IPA CsPbIBr2) and the CsPbIBr2 film treated
with isopropanol and thiourea (IPA-S CsPbIBr2) are illustrates in Fig. 1
(a), Fig. 1(b) and (c), which exhibits strikingly different morphologies
for three samples. The original film prepared by traditional technique
exhibits tinier grains with an incomplete coverage on the surface, as
shown in Fig. 1(a). As for the IPA CsPbIBr2 films produced with iso­
propanol antisolvent, Fig. 1(b) shows the huge grains. But a few of SnO2
also exposed, which can cause the short circuit inside the PSC. The IPA-S
CsPbIBr2 films as shows in Fig. 1(c), the perovskite produced with iso­
propanol antisolvent and thiourea, shows a near perfect surface
morphology with large grain size and no pinholes.
In order to confirm whether sulfur was doped into the perovskite
surface by isopropanol antisolvent, the IPA-S CsPbIBr2 films were
analyzed by energy dispersive spectroscopy (EDS), as shown in Fig. 2(a),
Fig.2(b) and Fig. S1. It can be clearly observed from Fig. 2(a) and (b)
that, the green light spots representing S ions uniformly cover the sur­
face of CsPbIBr2 films. It is proved that the S ions have been successfully
introduced into IPA-S CsPbIBr2 films surface by IPA-S antisolvent.
In order to understand the element composition and chemical state
of the surface of the IPA-S CsPbIBr2 films, the original and IPA-S
CsPbIBr2 films were measured by XPS, as shown in Fig. 2(c) and (d)
and Fig. S2. As shows in Fig. 2(c), compares with the original perovskite
film, The IPA-S CsPbIBr2 film has an obvious S 2p peak at the 162 eV. In
Fig. 2(d), both peaks of Pb 4f have obvious blue shift. These data prove
that the combination of S2− and Pb2+ increases the electron cloud
density of Pb, resulting in the blue shift of the characteristic peak of Pb
4f. According to previous literature, the formation of high-quality
CsPbIBr2 film was related to S2− introduced by IPA-S, because when
S2− and Pb2+ ions meet in CsPbIBr2 precursor solution film, the strong
Pb–S coordination will be formed, which promotes the uniform nucle­
ation of perovskite crystals, slows down the growth rate of perovskite
crystals, and increases the grain size [39,40].
X-ray diffraction (XRD) spectra are illustrated in Fig. 3(a), for
Fig. 1. SEM images of (a) original CsPbIBr2 film, (b) IPA CsPbIBr2 film, (c) IPA-S CsPbIBr2 film.
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Materials Science in Semiconductor Processing 150 (2022) 106940
recording the original, IPA and IPA-S CsPbIBr2 films in 2θ scope of
10◦ –50◦ . Due to the low concentration of the thiourea in the isopropanol
antisolvent, no obvious characteristic peak of sulfide can be found in
Fig. 3(a). The original, IPA and IPA-S CsPbIBr2 films have the same
properties α-CsPbIBr2 perovskite phase. Their (100), (110), (111) and
(200) lattice planes correspond to the characteristic diffraction peaks of
14.82, 21.09, 27.25 and 30.03, respectively [7,25,41–48]. Interestingly,
with the participation of the isopropanol antisolvent and thiourea, the
intensity of each characteristic peak is improved. The data demonstrates
that IPA-S CsPbIBr2 films exhibit the highest crystal orientation along
the out-of-plane each direction than original and IPA-S CsPbIBr2 films.
As the core layer of the PSCs, the optical properties of the perovskite
films directly affect the PCE of the PSCs. Therefore, we compared the
effects of IPA and IPA-S antisolvent on the light absorption of the
CsPbIBr2 films. As shown in Fig. 4(a), the UV–vis absorption spectra
show obvious differences among the original, IPA and IPA-S CsPbIBr2
films. It can be seen from the curve that, after antisolvent treatment with
IPA and IPA-S, the absorption band edge of the three kinds of CsPbIBr2
films did not change much, but the absorption intensity of the IPA-S
CsPbIBr2 film was significantly improved (the range less than 600
nm). In the Tauc plots Fig. 4(b), with the treatment of the isopropanol
and thiourea-isopropanol antisolvent, the bandgap decreases slightly. It
could be attributed that the IPA-S CsPbIBr2 films possessed fewer de­
fects, larger crystal grains, more uniform and denser perovskite film,
Thus, the CsPbIBr2 films can absorbs more light to produce photo­
generated carriers and effectively reduce recombination. This result is in
good agreement with the SEM images observed.
In order to detect the defect in the perovskite films, we then per­
formed the steady-state photoluminescence (PL) spectra. As shown in
Fig. 4(c), the signal responses based on the glass/perovskite structure
were recorded. The PL intensity increased significantly after antisolvent
treatment with isopropanol and thiourea-isopropanol, which is attrib­
uted to a reduction of the non-radiative recombination by passivated
defects and high crystallization quality on the surface of perovskite
films. In addition, a slight red shift of the PL peak (from 579 nm to 603
nm) was observed for the IPA-S-PSK perovskite films, which is the good
Q. He et al. Materials Science in Semiconductor Processing 150 (2022) 106940

Fig. 2. (a) SEM images of IPA-S CsPbIBr2 film, (b) EDS of sulfur on the surface of IPA-S CsPbIBr2 film; (c) The XPS spectra of S-2p of the original and IPA-S CsPbIBr2
film, (d) the XPS spectra of Pb-4f of the original and IPA-S CsPbIBr2 film.

voltage (J-V) characteristic curve of the original CsPbIBr2 PSCs, IPA

CsPbIBr2 PSCs and IPA-S CsPbIBr2 PSCs were presented in Fig. 5(a). The
IPA-S CsPbIBr2 PSCs has the highest photoelectric parameters among the
three kinds of PSCs, the PCE is 6.72%, with short-circuit current density
(Jsc) = 10.15 mA/cm2, open-circuit voltage (VOC) = 1.19V and Fill
Factor (FF) = 56.30%. However, the PCE of IPA and original CsPbIBr2
PSCs is only 5.97% and 5.25%. Fig. 5(b) shows the EQE spectra of the
original, IPA and IPA-S CsPbIBr2 PSCs. These curves display similar
trends, where the integrated current densities of the original, IPA and
IPA-S CsPbIBr2 PSCs are 8.45, 8.03 and 7.60 mA/cm2, respectively,
which agree with the Jsc values in the J− V curves. The results show that
the improvement of photoelectric parameters is due to the joint opti­
mization of the IPA-S CsPbIBr2 PSCs by antisolvent IPA and additive
thiourea. IPA as the antisolvent can effectively increase the grain size of
CsPbIBr2 film and reduce grain boundary defects; Thiourea as the ad­
ditive, in which S2− can effectively combine with the exposed Pb2− on
the CsPbIBr2 surface, passivate its surface defects, and further promote
the formation of pinhole free CsPbIBr2 film. Those reasons have been
verified in SEM, PL, UV–vis tests above.
In order to study the charge transfer dynamics in the PSCs, we
measured the electrochemical impedance spectroscopy (EIS) under dark
and open-circuit voltage (Voc) conditions. Fig. 5(c) shows the Nyquist
Fig. 3. (a) The XRD spectra of the original, IPA and IPA-S CsPbIBr2 film.
plot of the original, IPA and IPA-S PSCs, and the equivalent circuit model
was given in illustration. The EIS can be divided into two parts, low
agreement with the Tauc plots (Fig. 4(b)).
frequency and high frequency. As usually, the high frequency part
In order to explore the influence of IPA and IPA-S on the power
means the charge carrier transmission process, which is consisted of the
conversion efficiency (PCE) of the CsPbIBr2 PSCs, the current density –
charge transmission resistance (Rct) and the charge transmission

4
Q. He et al.
Fig. 4. (a) UV–vis absorbance, (b) The Tauc plots and (c) PL spectra of the original, IPA and IPA-S CsPbIBr2 film.
capacitance (Cct). The fewer the Rct means the stronger the charge
transmission ability. The low frequency part showed the recombination
process of the charge carrier, and it is composed of recombination
resistance (Rrec) and recombination capacitance (Crec). The larger Rrec
means the lower degree of carrier recombination. As the result showed
in Fig. 5(c) and Table S1, after the original PSCs was treated by IPA and
IPA-S respectively, the Rct of the PSCs was reduced from 348.8 to 288.2
and 246.3 Ω, and the Rre was increased from 860.1 to 1010.9 and
2023.7 Ω. The reduced Rct and the increased Rrec indicate that, after the
IPA and IPA-S treated, the PSCs can advance the charge transmission
ability and effectively inhibit the recombination of carriers. The
enhancement of charge transmission ability and the weakening of the
nonradiative recombination rate improve the PCE of the PSCs. These
results are caused by the IPA as an antisolvent can significantly promote
the crystallization quality of perovskite (as showed in the SEM images,
Fig. 1(c)), and the S2− can combine with the exposed Pb2+ on the
perovskite surface, so as to improve the crystallization quality, passivate
its defects and improved electronic transmission capability (as showed
in the SEM, XPS and PL, Figs. 1 and 4).
In addition to binding with Pb2+, S2− also have strong reducibility,
which can inhibit the PSCs failure caused by oxidation. As shown in
Fig. 5(d), in order to study the PSCs stability, we collected the PCE
changes of the three kinds PSCs within 10 days in the air of 40% hu­
midity. It is obvious that the original CsPbIBr2 PSCs and the IPA
CsPbIBr2 PSCs completely failed on the 5th and 6th day respectively,
while the IPA-S CsPbIBr2 PSCs still maintained 85% of the initial PCE on
the 10th day.
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Materials Science in Semiconductor Processing 150 (2022) 106940
4. Conclusion
The CsPbIBr2 perovskite cells (PSCs) treated with isopropanol (IPA)
antisolvent with thiourea has excellent photoelectric parameters and
good stability in the air. It shows large grain size and pinhole free
CsPbIBr2 film, compared with the original CsPbIBr2 film and the
CsPbIBr2 film treated only by IPA. The S2− introduced by thiourea can
combine with the exposed Pb2+ on the perovskite surface to effectively
passivate defects and reduce nonradiative recombination. These im­
provements have enabled us to prepare the carbon based CsPbIBr2 PSCs
with 6.79% champion PCE, which is nearly 30% higher than the original
carbon based CsPbIBr2 PSCs. In addition, due to the strong reducibility
of S2− , the carbon based CsPbIBr2 PSCs treated with isopropanol anti­
solvent added with thiourea can continue to work in air with 40%
relative humidity, and the efficiency can remain 85% within 10 days. In
order to improve the performance and stability of the all-inorganic PSCs,
this paper provides a non-toxic, environmentally friendly and effective
scheme.
5. Notes
The authors declare that they have no conflict of interest.
CRediT authorship contribution statement
Qingchen He: Conceptualization, Data curation, Investigation,
Methodology, Project administration, Software, Writing – original draft.
Q. He et al.
Fig. 5. (a) J–V characteristic curves (under reverse scan), (b) EQE spectra along with integrated current densities, (c) Nyquist plot (under dark at Voc) of the original,
IPA and IPA-S CsPbIBr2 PSCs.; (d) The stability under 40% RH in the air for the original, IPA and IPA-S CsPbIBr2 PSCs.
Haiming Zhang: Conceptualization, Project administration, Supervi­
sion, Validation, Visualization, Writing – review & editing. Siqi Han:
Data curation, Supervision. Yuwen Xing: Data curation. Yujie Li:
Formal analysis. Xianjing Zhang: Formal analysis. Rufeng Wang:
Formal analysis.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
No data was used for the research described in the article.
Acknowledgements
This work was funded by The Science & Technology Development
Fund of Tianjin Education Commission for Higher Education
（2019ZD23）.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.mssp.2022.106940.
6
Materials Science in Semiconductor Processing 150 (2022) 106940
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