RES EARCH

SOLAR CELLS methyl or chloride in the para position of the

benzene ring opposite to the sulfonate func-
Improved charge extraction in inverted perovskite tional group [4-methylbenzenesulfonate (4CH3-
BZS) and 4-chlorobenzenesulfonate (4Cl-BZS)]
solar cells with dual-site-binding ligands (Fig. 1A). 4CH3-BZS and 4Cl-BZS have lengths
of 6.14 and 6.37 Å, respectively. We compared
Hao Chen1,2†, Cheng Liu1†, Jian Xu2†, Aidan Maxwell2†, Wei Zhou3†, Yi Yang1, Qilin Zhou3, the formation energies of two configurations,
Abdulaziz S. R. Bati1, Haoyue Wan2, Zaiwei Wang2, Lewei Zeng2, Junke Wang2, Peter Serles4, Yuan Liu1, one in which the ligands were oriented perpen-
Sam Teale2, Yanjiang Liu2, Makhsud I. Saidaminov5, Muzhi Li6, Nicholas Rolston6, Sjoerd Hoogland2, dicular to the perovskite surface (Conf-perp;
Tobin Filleter4, Mercouri G. Kanatzidis1, Bin Chen1*, Zhijun Ning3*, Edward H. Sargent1,2,7* Fig. 1B) and another in which the ligands
adopted a parallel orientation with respect
Inverted (pin) perovskite solar cells (PSCs) afford improved operating stability in comparison to their to the perovskite surface (Conf-para; Fig. 1C).
nip counterparts but have lagged in power conversion efficiency (PCE). The energetic losses responsible Although Conf-perp was more energetically
for this PCE deficit in pin PSCs occur primarily at the interfaces between the perovskite and the favorable for BZS and 4CH3-BZS, Conf-para
charge-transport layers. Additive and surface treatments that use passivating ligands usually bind to a was energetically more favorable for 4Cl-BZS
single active binding site: This dense packing of electrically resistive passivants perpendicular to the because of the additional Pb2+ surface bind-

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surface may limit the fill factor in pin PSCs. We identified ligands that bind two neighboring lead(II) ing afforded by the Cl functional group (Fig. 1D)
ion (Pb2+) defect sites in a planar ligand orientation on the perovskite. We fabricated pin PSCs that would enable dual-site Pb2+ passivation.
and report a certified quasi–steady state PCE of 26.15 and 24.74% for 0.05– and 1.04–square We also investigated the effects of ligand ori-
centimeter illuminated areas, respectively. The devices retain 95% of their initial PCE after 1200 hours entation on charge transfer at the perovskite-
of continuous 1 sun maximum power point operation at 65°C. ETL interface by examining fullerene (C60),
which is widely used as an ETL in pin PSCs

T
and is known to induce energetic losses in de-
he certified power conversion efficiency lished (17, 18). However, these ligands bind vices (11, 12, 34, 35). Analysis of the calculated
(PCE) of perovskite solar cells (PSCs) has at a single active binding site to the perov- charge density difference (Fig. 1E and fig. S1)
reached an impressive 25.7% (1). Never- skite structure, and this has the potential to provided evidence that 4Cl-BZS, when absorbed
theless, the most-efficient PSCs, fabri- produce dense packing of passivants aligned on the perovskite layer, established a notably
cated in the nip architecture, have yet to perpendicular to the surface, introducing an stronger binding strength with the C60 layer
achieve the needed operating stability under unwanted resistive barrier between the perov- [adsorption energies (Eads) = −0.85 eV] in
accelerated aging tests (1, 2). Inverted (pin) skite and the electron transport layer (ETL) contrast to BZS (Eads = −0.46 eV) and 4CH3-
PSCs, which do not rely on p-type dopants in (16, 19–25). We sought routes to passivate un- BZS (Eads = −0.39 eV) (36). Fracture energy
their hole-transporting layers (3–7), have dercoordinated Pb2+ at the surfaces and grain (Gc) results show that 4Cl-BZS increases the
seen progress but, until now, still lag behind boundaries of the perovskite with passivator mechanical strength of the perovskite-C60
their nip counterparts: Their stabilized PCE ligands aligning parallel to the perovskite sur- interface (fig. S2) (37).
has so far reached only 25.1% (8). The inter- face instead.
faces between the perovskite and the charge- Ligand-perovskite binding characterization
transport layers limit the PCE of pin cells (9–11) Theoretical investigations To explore interactions between perovskite
through band misalignment (12) and energy- We began by considering candidate molecules and BZS ligands, we began by adding each
level pinning (11). These problems are ag- that contain a benzene ring because its flat ligand directly into the precursor solutions and
gravated by the presence of surface defects. structure is expected to lie parallel to a surface spin-coating Cs0.05FA0.85MA0.1PbI3 perovskite
For example, undercoordinated Pb2+ ions compared with the case of linear-chain ligands thin films, where FA is formamidinium and
(13–15) result in nonradiative recombination (21). To enable strong binding with perovskite MA is methylamine. Time-of-flight secondary
at the perovskite–charge transport layer in- surfaces, we considered both –PO32− and –SO3− ion mass spectrometry (TOF-SIMS) of untreated
terface, which limits photovoltage and fill functional groups, each of which is reported to (control) and treated films showed that BZS,
factor (FF). coordinate strongly with Pb2+ (14, 26). Because 4CH3-BZS, and 4Cl-BZS were all concentrated
Surface passivation of the perovskite active benzenephosphonates are not readily availa- near the top (ETL-facing) surface of the perov-
layer is used to suppress interface nonradia- ble, we focused on available sulfonates (27–33). skite film (fig. S3). This result, combined with
tive recombination (14, 16). The efficacy of bulk We prioritized end functional groups that have x-ray diffraction (XRD) patterns of control and
additives as well as solution-based treatments a high number of oxygen atoms, a feature treated perovskite films that showed no dis-
with ammonium ligands is now well estab- recently reported to correlate positively with cernable peak-shifting after treatment (fig.
strong binding (26). S4), indicated that the ligands did not enter
1
We then evaluated steric constraints, seek- the lattice but rather diffused toward the top
Department of Chemistry, Northwestern University, Evanston,
IL 60208, USA. 2Department of Electrical and Computer
ing a ligand sufficiently long that it could bind surface during film crystallization. Scanning
Engineering, University of Toronto, Toronto, ON M5S 1A4, at multiple surface Pb sites, these being ~6.3 Å electron microscopy (SEM) images of perov-
Canada. 3School of Physical Science and Technology, apart in the case of formamidinium (FA)–based skite films with additives are presented in fig.
ShanghaiTech University, Shanghai, China. 4Department of
Mechanical and Industrial Engineering, University of Toronto,
perovskites. These considerations pointed to S5 and illustrate that the perovskite films (both
Toronto, ON M5S 3G8, Canada. 5Department of Electrical benzenesulfonate (BZS) ligands and their de- additives and controls) exhibit substantially
and Computer Engineering, University of Victoria, Victoria, BC rivatives because these molecules have a length uniform morphology.
V8P 5C2, Canada. 6Ira A. Fulton Schools of Engineering,
of ~5.7 Å. We used x-ray photoelectron spectroscopy
Arizona State University, Tempe, AZ 85281, USA. 7Department
of Electrical and Computer Engineering, Northwestern We used density functional theory (DFT) (XPS) to check for possible evidence of inter-
University, Evanston, IL 60208, USA. calculations to investigate how the molecular action between the additives and perovskite.
*Corresponding author. Email: [email protected] (B.C.); structure of the ligand affects orientation. We We observed a shift of the Pb 4f XPS peaks to
[email protected] (Z.N.); ted.sargent@northwestern.
edu (E.H.S.) considered three ligands, one with no addi- a lower binding energy for each treated film
†These authors contributed equally to this work. tional functional group (BZS) and two with compared with the peaks of controls (Fig. 2A).

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Fig. 1. DFT studies of ligand binding and predicted orientation. (A) Structure parallel orientation (Conf-para) on the perovskite surface. (D) Formation energy
and electrostatic potential of BZS, 4CH3-BZS, and 4Cl-BZS ligands. (B) Atomic difference between parallel and perpendicular ligand-surface orientations (EConf-para −
structures of ligand adsorbed in a perpendicular orientation (Conf-perp) on EConf-perp). (E) The adsorption energies (Eads) of C60 with different molecules
the perovskite surface. (C) Atomic structures of ligand adsorbed in a planar or (BZS, 4CH3-BZS, and 4Cl-BZS) adsorbed on the perovskite surface.

We saw evidence of interaction between Cl and We observed an increase in PL quantum yield 4PACz] revealed a substantial improvement
Pb in 4Cl-BZS–treated perovskite from both (PLQY) for each of the treated films and the full after 4Cl-BZS treatment—5% for 4Cl-BZS com-
XPS spectra (Fig. 2B) and nuclear magnetic device stack (Fig. 2C), with 4Cl-BZS exhibiting pared with 0.6% for the control, corresponding
resonance spectra (fig. S6). a twofold increase in PLQY (41%) compared to 1.17 and 1.1 V in QFLS for 4Cl-BZS and the
with control films (20%), which corresponded control device, respectively. This improvement
Optoelectronic characterization of perovskite to a projected 20-mV increase in quasi-Fermi was consistent with reduced interface losses.
films and device stacks level splitting (QFLS). The PLQY of full-device Time-resolved photoluminescence (TRPL) re-
To evaluate the passivation efficacy of each stacks [FTO/SAMs/perovskite/C60, where FTO vealed a similar increase in carrier lifetimes
ligand, we studied photoluminescence (PL) is fluorinate tin oxide and SAMs (self-assembled after treatment. Specifically, 4Cl-BZS–treated
of neat control and treated perovskite films. monolayers) are mixtures of 2PACz and Me- films exhibited a weighted-average lifetime of

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Fig. 2. Surface coordination and passivation of perovskite films. (A) Pb 4f perovskite/C60) with and without treatment. (D) TRPL lifetimes of neat
XPS spectra of control and treated perovskite surfaces. a.u., arbitrary units. control and treated perovskite films. The lifetimes for each trace were calculated
(B) Cl 2p XPS spectra of pure 4Cl-BZS film compared with spectra of perovskite using a biexponential decay model and can be found in table S1. (E) Differential
treated with 4Cl-BZS. (C) PLQY of neat control and treated perovskite films carrier lifetimes extracted from the TRPL spectrum (fig. S7). (F) Transient
on quartz substrates and PLQY results for full device stacks (FTO/SAMs/ photocurrent (TPC) measurements of control and treated devices.

3.0 ms compared with 0.6 ms for the control the sharpness of the rise implied the speed of trol devices had a PCE of 24%, whereas the
film (Fig. 2D and table S1). the electron transfer from perovskite to C60. 4Cl-BZS–treated devices exhibited a PCE of
We fabricated partial and full perovskite/ Transient photocurrent measurements of full 26.3% (fig. S12). Analysis of device statistics
ETL device stacks to probe interface recom- device stacks in which we used mixed SAMs for both control and 4Cl-BZS–treated PSCs re-
bination and charge transfer. First, we con- as the hole-transport layer (see methods) re- vealed a substantial enhancement in PCE, pri-
ducted TRPL measurements of perovskite/C60 vealed a similar trend. Both BZS and 4CH3- marily by increased open-circuit voltage (VOC).
stacks, wherein decay was dictated by non- BZS resulted in slower photocurrent decay, Additionally, 4Cl-BZS–treated PSCs showed
radiative surface-bulk recombination (mono- whereas 4Cl-BZS treatment led to faster photo- a much higher FF compared with BZS- and 4CH3-
exponential decay), radiative recombination current decay (Fig. 2F). This observation sug- BZS–treated PSCs. We attribute this improvement
(second-order decay), and charge extraction gested that electron extraction became more in FF to enhanced charge extraction in 4Cl-BZS–
effects, which could be distinguished if the efficient. Ultraviolet photoelectron spectroscopy treated PSCs (Fig. 3B and figs. S13 and S14).
time constants for each process differed suf- (UPS) revealed an increased conduction band We also evaluated the effectiveness of the ad-
ficiently (38). The first interval at shorter times offset with C60 that was caused by a Fermi-level ditive change with a stronger or weaker donat-
was dominated by the transfer of electrons upshift after BZS and 4CH3-BZS treatment, ing group, namely 4F-BZS, 4Br-BZS, and 4I-BZS.
from the bulk into the C60, and the second in- whereas 4Cl-BZS caused a Fermi-level down- Notably, 4F-BZS exhibits a more-negative av-
terval at longer delay times was dominated shift and reduced conduction band offset (figs. eraged electrostatic potential, whereas 4I-BZS
by interfacial recombination (39). The sharp S8 and S9). This trend was further confirmed displays a more-positive averaged electrostatic
drop in emission for 4Cl-BZS/C60 indicated by kelvin probe force microscopy (KPFM) mea- potential (fig. S15). We posit that a stronger
efficient electron transfer at the interface, and surements (fig. S10 and table S2) and DFT donating group, such as Cl or F, is beneficial in
the longer second-order decay time was indic- calculations (fig. S11). providing dual-site defect passivation. Because
ative of a reduced trap density compared with 4F-BZS, 4Cl-BZS, and 4I-BZS are not readily
BZS and 4CH3-BZS (fig. S7). This effect of this Inverted perovskite solar cells available, we used the structurally similar mol-
reduction was especially evident in fits to the Using 4Cl-BZS–treated perovskite, we fabricated ecules 4-fluorobenzenesufonic acid (4F-BZSA)
TRPL traces to compute the differential lifetime inverted PSCs with the structure FTO/SAMs/ and 4-iodobenzenesufonic acid (4I-BZSA) in
as t = –{d ln[f(t)]/dt}–1 (Fig. 2E), where f(t) is the perovskite/C60/SnOx/Ag (Fig. 3A). The thick- our devices (fig. S16). Notably, treatments with
time-dependent PL photon flux, because ness of the perovskite layer was 900 nm. Con- 4F-BZSA resulted in comparable PCE as in the

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Fig. 3. Photovoltaic performance and stability of inverted solar cells. 0.05-cm2 device (fig. S15). (E) Newport-certified QSS J-V curve of the champion
(A) Cross-sectional SEM image of the device structure. (B) PCE statistics for 1.04-cm2 device (fig. S16). (F) Summary of published nip and pin PSC
30 control and 4Cl-BZS–treated devices. The center line represents the median, performances in recent years. (G) ISOS-D-2I device stability during storage
box limits are upper and lower quartiles, and whiskers are minimum and at 85°C for 1500 hours. (H) MPP stability tracking of encapsulated control and
maximum values; the vertical curved lines represent data distribution. (C) J-V 4Cl-BZS–treated devices under simulated 1-sun illumination at 50% relative
curves of the 4Cl-BZS–treated device with bimolecular passivation. The inset humidity (RH) and a heatsink temperature of 65°C. The 4Cl-BZS–treated device
shows the stabilized PCE. (D) Newport-certified QSS J-V curve of the champion retains 95% of its initial efficiency after 1200 hours of operation.

case of 4Cl-BZS, and 4I-BZSA also showed an increased the PCE of 4Cl-BZS–treated devices accredited independent photovoltaic calibra-
improved PCE compared with controls. from 26.3 to 26.9% and featured a VOC of 1.18 V, tion laboratory (Newport) for certification. The
We then added the bimolecular surface pas- FF of 86.2%, and short-circuit current density devices achieved certified stabilized quasi–
sivation (BMP) approach, based on 3-(methylthio) (JSC) of 26.4 mA cm−2 (Fig. 3C). Statistics of steady state (QSS) PCEs of 26.15 and 24.74%,
propylamine hydroiodide (3MTPAI) and propane- photovoltaic parameters for devices with bi- respectively (Fig. 3, D and E, and figs. S21 and
1,3 diammonium iodide (PDAI2), reported in (8). molecular passivation revealed additional im- S22). These reported pin PSC PCEs surpass the
This strategy has been reported to provide a provements in both VOC and PCE (fig. S18). record nip device performance reported in re-
combination of chemical and field-effect passi- The bandgap of the pin PSCs was taken from cent years (Fig. 3E and tables S3 and S4).
vation (see methods). The PLQY of full-device external quantum efficiency measurements Next, we sought to test the thermal stability
stacks (FTO/SAMs/perovskite/BMP/C60) indi- as 1.53 eV (figs. S19 and S20). We sent devices of the 4Cl-BZS–treated PSCs following proto-
cated a further improvement after the BMP with active areas of 0.05 and 1.04 cm2 to a Na- cols established by the International Sum-
treatment (fig. S17). The combined treatment tional Renewable Energy Laboratory (NREL)– mit on Organic Photovoltaic Stability (ISOS)

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protocol ISOS-D-2I, in which encapsulated mixed halide devices as well as 1.25-eV narrow- 37. M. Li et al., Energy Adv. 3, 273–280 (2024).
devices were subjected to dark storage at 85°C bandgap mixed Pb-Sn PSCs, which are com- 38. A. Al-Ashouri et al., Science 370, 1300–1309 (2020).
39. T. Li et al., Nat. Energy 8, 610–620 (2023).
and tested periodically. 4Cl-BZS–treated PSCs positions of interest in all-perovskite tandem
retained 95% of their initial efficiency after solar cells. In each case, we observed an increase AC KNOWLED GME NTS
1500 hours of storage at 85°C (Fig. 3G). To in PCE after 4Cl-BZS treatment (fig. S24). Funding: This work was supported in part by the Ontario Research
evaluate operating stability further, we then Fund-Research Excellence program (ORF7-Ministry of Research
RE FERENCES AND NOTES and Innovation, Ontario Research Fund-Research Excellence
also carried out ISOS-L-3 testing, in which en- Round 7). This work was also supported by the Natural Sciences
1. J. Park et al., Nature 616, 724–730 (2023).
capsulated devices were subjected to contin- 2. Y. Zhao et al., Science 377, 531–534 (2022). and Engineering Council of Canada and the Vanier Canada Graduate
uous 1-sun equivalent illumination using a 3. H. Chen et al., Adv. Mater. 31, 1903559 (2019). Scholarship. A.S.R.B. acknowledges support from King Abdullah
University of Science and Technology (KAUST) through the
ultraviolet-free white light-emitting diode 4. B. Chen et al., Adv. Mater. 33, e2103394 (2021).
5. Q. Jiang et al., Nature 611, 278–283 (2022). Ibn Rushd Postdoctoral Fellowship Award. This research was made
(LED) and held at the maximum power point possible by the US Department of Energy’s Office of Energy
6. S. You et al., Science 379, 288–294 (2023).
(MPP) voltage, at 50% relative humidity and 7. S. M. Park et al., Nature 624, 289–294 (2023). Efficiency and Renewable Energy (EERE) under the Solar Energy
a heatsink temperature of 65°C (Fig. 3H). 8. C. Liu et al., Science 382, 810–815 (2023). Technologies Office award no. DE-EE0008753. M.G.K. is supported
9. S. Cacovich et al., Nat. Commun. 13, 2868 (2022). by the US Department of Energy, Office of Science, Basic Energy
4Cl-BZS–treated PSCs achieved a T95 (the time Science, under award number DE-SC-0012541 (fundamental studies
10. M. Stolterfoht et al., Nat. Energy 3, 847–854 (2018).
it takes for the device’s PCE to drop to 95% of 11. J. Warby et al., Adv. Energy Mater. 12, 2103567 (2022). on metal halides). This work was partially funded by the Trienens
the initial value) of 1200 hours after contin- 12. M. Stolterfoht et al., Energy Environ. Sci. 12, 2778–2788 Institute for Sustainability and Energy at Northwestern University.
(2019). Z.N. acknowledges support from the National Key Research

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uous MPP tracking at 65°C, whereas control Program (2021YFA0715502) and the National Science Fund of China
13. X. Gu, W. Xiang, Q. Tian, S. F. Liu, Angew. Chem. Int. Ed. 60,
devices dropped from an initial efficiency of 23164–23170 (2021). (61935016, 22175118, and 92056119), as well as the Double
22 to 18.7% after 1200 hours (table S5). Fur- 14. C. Li et al., Science 379, 690–694 (2023). First-Class Initiative Fund of ShanghaiTech University. This work
15. T. Yang et al., Nat. Commun. 14, 839 (2023). made use of the SPID, EPIC, and Keck-II facilities of Northwestern
thermore, 4Cl-BZS–treated PSCs achieved a University’s NUANCE Center, which has received support from
16. S. M. Park et al., Science 381, 209–215 (2023).
T87 of 540 hours after continuous MPP track- 17. F. Gao, Y. Zhao, X. Zhang, J. You, Adv. Energy Mater. 10, the SHyNE Resource (NSF ECCS-2025633). This work was supported
ing at 85°C (fig. 23). 1902650 (2020). by the International Institute of Nanotechnology, Northwestern
18. J. Xia et al., Energy Environ. Mater. 6, e12296 (2023). University, and Northwestern’s MRSEC program (NSF DMR-1720139).
Author contributions: Conceptualization: H.C.; Device fabrication:
Discussion 19. M. G. La-Placa et al., ACS Energy Lett. 4, 2893–2901
(2019). H.C.; Film fabrication and characterization: H.C., C.L., W.Z., Y.Y.;
We began this study with the view that dense 20. S. M. Park, A. Abtahi, A. M. Boehm, K. R. Graham, ACS Energy TPC and TOF-SIMS: Y.Y., C.L.; DFT calculations: J.X.; UPS and XRD
measurements: W.Z., Q.Z.; SEM and XPS measurements: C.L.,
packing of passivator ligands perpendicular Lett. 5, 799–806 (2020).
21. H. Chen et al., Nat. Photonics 16, 352–358 (2022). Y.Y., A.S.R.B., Ya.L.; KPFM measurements: Y.Y., P.S.; PL, TRPL, PLQY
to the perovskite-C60 interface may increase measurements: A.M., Y.Y., C.L., H.W., Z.W., L.Z., J.W., Yu.L., S.T.;
22. J. Chakkamalayath, N. Hiott, P. V. Kamat, ACS Energy Lett. 8,
resistance and that this could potentially be 169–171 (2023). Fracture energy measurements: M.L., N.R.; Writing – original
addressed by instead introducing ligands 23. C. A. R. Perini et al., Adv. Mater. 34, e2204726 (2022). draft: A.M.; Writing – review and editing: H.C., C.L., J.X., B.C., M.I.S.,
24. K. Ma et al., Adv. Mater. 33, e2100791 (2021). S.H., T.F., M.G.K., Z.N., E.H.S.; Supervision: B.C., Z.N., E.H.S.
prone to align in a planar orientation relative Competing interests: B.C., H.C., and E.H.S. are filing a patent
25. Q. Jiang et al., Nat. Photonics 13, 460–466 (2019).
to the perovskite surface. The interaction of 26. J. Xu et al., Nat. Mater. 22, 1507–1514 (2023). based on this work. The other authors declare no competing
4Cl-BZS with undercoordinated Pb2+ ions re- 27. S. Kajal et al., Chem. Eng. J. 451, 138740 (2023). interests. Data and materials availability: All data are available in
28. Y. Hao et al., J. Mater. Chem. A Mater. Energy Sustain. 10, the main text or the supplementary materials. License
duces the surface defect density and mini- information: Copyright © 2024 the authors, some rights reserved;
13048–13054 (2022).
mizes the energetic mismatch between the 29. H. Wang et al., J. Mater. Chem. C Mater. Opt. Electron. Devices exclusive licensee American Association for the Advancement of
perovskite and C60. Our study indicates that 11, 13518–13525 (2023). Science. No claim to original US government works. https://www.
science.org/about/science-licenses-journal-article-reuse
the approach was effective in increasing pin 30. R. Chen et al., J. Am. Chem. Soc. 143, 10624–10632 (2021).
31. K. Liu et al., Joule 4, 2404–2425 (2020).
PSC performance, bringing it into the range of SUPPLEMENTARY MATERIALS
32. J. C. Hamill Jr. et al., J. Phys. Chem. C Nanomater. Interfaces
that achieved in the nip configuration. Our ap- 124, 14496–14502 (2020). science.org/doi/10.1126/science.adm9474
proach retains the benefits of the 65°C 1-sun 33. K. Hills-Kimball, H. Yang, T. Cai, J. Wang, O. Chen, Adv. Sci. Materials and Methods
(Weinh.) 8, 2100214 (2021). Figs. S1 to S24
MPP operating stability seen in pin PSCs. Tables S1 to S5
34. H. Chen et al., Nature 613, 676–681 (2023).
To test whether our approach worked in a References (40–54)
35. J. Liu et al., Science 377, 302–306 (2022).
range of perovskite compositions, we fabri- 36. B. Li et al., ACS Appl. Mater. Interfaces 10, 32471–32482 Submitted 14 November 2023; accepted 14 March 2024
cated 4Cl-BZS–treated 1.78-eV wide-bandgap (2018). 10.1126/science.adm9474

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