Gamma Rays Induced Decomposition in the Triple-Cation Perovskite

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Energy Conversion and Storage; Plasmonics and Optoelectronics

Gamma Rays Induced Decomposition in the Triple-Cation Perovskite Solar Cells Aleksandra G. Boldyreva, Azat F. Akbulatov, Sergey Tsarev, Sergey Yurevich Luchkin, Ivan S Zhidkov, Ernst Zagidovich Kurmaev, Keith J. Stevenson, Vladimir Petrov, and Pavel A Troshin J. Phys. Chem. Lett., Just Accepted Manuscript • DOI: 10.1021/acs.jpclett.8b03222 • Publication Date (Web): 08 Jan 2019 Downloaded from http://pubs.acs.org on January 9, 2019

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The Journal of Physical Chemistry Letters

Gamma Rays Induced Degradation in the TripleCation Perovskite Solar Cells Aleksandra G. Boldyreva†, Azat F. Akbulatov‡, Sergey A. Tsarev†, Sergey Yu. Luchkin†, Ivan S. Zhidkov&, Erst Z. Kurmaev&,#, Keith J. Stevenson†, Vladimir G. Petrov§, Pavel A. Troshin*,†, ‡

† Skolkovo

‡ Institute

Institute of Science and Technology, Nobel street 3, Moscow, 143026, Russia.

for Problems of Chemical Physics of the Russian Academy of Sciences (ICP RAS),

Semenov prospect 1, Chernogolovka, 142432, Russia &

Institute of Physics and Technology, Ural Federal University, Mira 9 str., 620002

Yekaterinburg, Russia #

M.N.Mikheev Institute of Metal Physics of Ural Branch of Russian Academy of Sciences, S.

Kovalevskoi 18 str., 620108 Yekaterinburg, Russia § Lomonosov

Moscow State University, Lelinsky Gory, Moscow, 119991, Russia

Corresponding Author *E-mail:

[email protected]. Tel: +7-496-522-1418

ACS Paragon Plus Environment

1


ABSTRACT

We report on the impact of gamma radiation (0-500 Gy) on the triple cation Cs0.15MA0.10FA0.75Pb(Br0.17I0.83)3 perovskite solar cells. A set of experiments was designed to reveal the individual contributions of the hole-collecting bottom electrode, perovskite absorber and electron transport layer (ETL) to the overall solar cell degradation under the radiation exposure. We show that Glass/ITO/PEDOT:PSS hole-collecting electrode withstands 500 Gy dose without any losses in the solar cell performance. On the contrary, the perovskite absorber films and PC61BM ETL are very sensitive to gamma rays as can be concluded from the radiationinduced decay of the solar cell efficiency by ~32-41%. Red shift of the perovskite emission bands and strong enhancement of the photoluminescence suggest that gamma rays induce phase segregation of iodine-rich and bromine-rich domains, which represents the first reported example of the radiation-induced Hoke effect. The revealed here degradation pathway emphasizes the need for developing a new generation of metal halide absorbers and ETL materials with improved radiation stability to enable potential space applications of perovskite photovoltaics.

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Since the emergence of the space industry, different types of solar cells have been used as the main electrical energy source to power spacecrafts and satellites. Solar irradiation in space is substantially stronger than on Earth, and it has no disturbance in a form of clouds, which makes it a more consistent and reliable energy source to convert photons to electrical energy. However, high-energy particles and radiation sources, such as protons, electrons, X-rays and gamma rays from such entities as Sun flares and galactic radiation can react with and evenly destroy conventional semiconductor materials.1,2 Severe radiation-induced degradation effects were documented for solar cells based on Si, A3B5 materials such as GaAs alone or in tandems with other absorbers such as InP.2-5 A considerable effort in modelling the aging effects6-8 and developing the appropriate shielding technologies9-11 allowed one to suppress significantly the radiation-induced degradation of photovoltaic panels, while the problem is still not solved so far.12 Recently, the list of materials that can compete with silicon in terms of photovoltaic performance was extended by perovskites representing complex lead halides, which currently deliver power conversion efficiencies of up to 22-23.3%.13,14 There are still very few works dedicated to understanding the radiation stability of perovskites, especially focusing on longterm stability effects.15 While it has been reported in 2018 that hybrid perovskite solar cells have a superior radiation stability,16 the study found that electron beams with the energy of 1 MeV did not change the structure and characteristics of the perovskite solar cells, which leads to circumspect conclusions. In a follow on study, it was shown that CH3NH3PbBr3 solar cells are more resistant to proton irradiation than Si-based panels.17 Moreover, the perovskite films demonstrated a “self-healing effect” reflected in the passivation of defects induced by proton irradiation (63 MeV) within two weeks after exposure. Notably, the researchers working in this


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field often neglect other types of ionizing radiation, such as X-rays and γ-rays. While the influence of γ-rays on Si solar cells was already explored,18,19 to the best of our knowledge, there are still no reports on the gamma radiation tolerance of perovskite solar cells. Herein we explore the impact of γ-rays on the chemical composition, film morphology, crystal structure and photovoltaic performance of the “triple-cation” Cs0.15MA0.10FA0.75Pb(Br0.17 I0.83)3. perovskite solar cells. Since perovskite solar cells represent multilayer stacks, each of the layers can potentially contribute to the device degradation. Therefore, we systematically explored the influence of γ-rays to the glass/ITO/PEDOT:PSS electrodes, perovskite absorber material and PC61BM electron transport layer. Fig. 1 shows the architectures of three sets of samples used in this work and the general methodology of the performed experiments.

Figure 1. Architecture and protocol of investigated samples and general methodology of the experiment investigation: (a) Glass/ITO/PEDOT:PSS, (b) Glass/ITO/PEDOT:PSS/perovskite, (с) Glass/ITO/PEDOT:PSS/perovskite/PC61BM.


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Radiation doses in the range of 0-500 Gy were applied to the samples since 100-1000 Gy represents a typical stability benchmark for satellites working at low and middle equatorial orbits.9 First, we checked the radiation stability of the glass substrates with the hole-collecting bottom electrodes glass/ITO/PEDOT:PSS (Fig. 1a) by exposing the samples to 150, 300 and 500 Gy doses. Then the sets of reference non-exposed samples and the experimental samples exposed to the radiation were processed further in one batch under the same conditions to fabricate the complete solar cell architectures. Briefly, perovskite and then PC61BM layers were deposited by spin-coating inside the nitrogen glove box followed by deposition of Ag contacts by thermal evaporation in high vacuum (details given in Experimental). The mixed “triple-cation” Cs0.15MA0.10FA0.75Pb(Br0.17I0.83)3 perovskite formulation (designated as “perovskite” below) was chosen because it shows high solar cell efficiencies and superior operation stability according to the available literature data.20-23 Notably,

the

devices

fabricated

using

exposed

and

the

reference

non-exposed

glass/ITO/PEDOT:PSS samples demonstrated nearly the same power conversion efficiencies (PCEs) of about 9.5-10.5% (Fig. S1, Supporting information, SI). The photovoltaic characteristics of all the samples were within the standard experimental data deviation window and showed no correlation with the radiation dose. These results allowed us to conclude that the glass substrate with the bottom ITO/PEDOT:PSS hole-collecting electrode is fully stable with respect to the radiation and, therefore, should not contribute to the device degradation. The second set of samples (Fig. 1b) exposed to gamma rays comprises the perovskite layer deposited on top of the glass/ITO/PEDOT:PSS stacks. Since the lead halide complexes form crystalline films, first we have applied X-ray diffraction (XRD) to check for any phase composition changes caused by gamma radiation. Both exposed and reference samples (Fig. S2,


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SI) were encapsulated by spin-coating polystyrene films inside the glove box and then were measured in ambient atmosphere for 10-15 min. It should be noticed that XRD pattern of the analyzed material matches well the pattern of previously reported (MAPbBr3)0.15(FAPbI3)0.85 perovskite showing differences only in the peak intensities probably due to different textural effects.24 Therefore, the (MAPbBr3)0.15(FAPbI3)0.85 XRD pattern was used as a reference one to analyze the experimental patterns of the perovskite films obtained in this work. XRD data presented in Fig. S2a (SI) show that gamma rays have no real impact on the phase purity of the perovskite films. No additional peaks indicating the appearance of the decomposition products (e.g. PbI2 or metallic Pb) or some phase transitions effects were observed. Moreover, there were essentially no changes in the XRD patterns of the glass/perovskite samples exposed to high doses of gamma rays (up to 5000 Gy, Fig. S2b, SI), which suggested that the triple-cation perovskite formulation investigated in this work is resistant to radiation. These XRD data were fully in line with the results of the XPS measurements. The XPS survey spectra (Fig. S3a) of all exposed samples were virtually identical and matching the spectrum of the pristine perovskite. Zooming the N 1s and Pb 4f7/2 signatures also showed almost no impact of the radiation with except for some band broadening observed for the sample exposed to the highest dose of 5000 Gy. This peak broadening might be related to some partial decomposition of the material (which is unlikely considering the XRD and optical spectroscopy data, see below) or to the radiation-induced gradients in the composition of the material (e.g. phase separation of I-rich and Br-rich domains). Thus, the main message provided by the XPS data is a good radiation stability of the used triple-cation perovskite formulation.


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Scanning probe microscopy was used to explore a potential impact of gamma radiation on the surface morphology and electronic properties of the perovskite films. In particular, the contact potential (surface potential) was measured by 2-pass amplitude modulated Kelvin Probe Force Microscopy

(AM-KPFM).

The

topography

and

surface

potential

images

for

the

glass/ITO/PEDOT:PSS/perovskite samples (exposed 500 Gy and reference) are shown in Fig. 2.

Figure 2. Surface potential (a, b) and topography (c,d) images of the reference (a,c) and exposed to 500 Gy (b, d) Glass/ITO/PEDOT:PSS/perovskite samples. Gamma radiation induced a minor change in the surface work function of the films from 4.67 eV to 4.72 eV, which might be related to the formation of the acceptor-type defects or ion vacancies. Topography images show that the samples exposed to 500 Gy have considerably larger grains (15 nm vs. 10 nm in non-exposed samples) and rougher surface (22 nm vs. 18 nm). We believe that radiation induces a crystallization of the perovskite material leading to the growth of the grains in the samples and increase in the film roughness though this hypothesis requires more systematic study. The effect of gamma radiation on the optical properties of the perovskite films was investigated by monitoring their absorption (UV-vis) and photoluminescence (PL) spectra as a


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function of the radiation dose. The UV-vis spectra did not noticeably change with exposure to gamma radiation. In particular, no notable radiation-induced change in the relative intensity of the existing or appearance of any new absorption features were observed even when the doses were as high as 2500-5000 Gy (Fig. S4, SI). On the contrary, PL spectra of the perovskite films revealed a considerable enhancement in the intensity of the emission bands, significant changes in their shape and notable shifts (by ~5 nm) of the maxima towards longer wavelengths following the increase in the radiation dose (Fig. 3a). In particular, the sample exposed to 500 Gy demonstrated unsymmetrical emission band with more than twice higher intensity (especially in the 785-820 nm range) as compared to the spectrum of the pristine sample. Moreover, exposing the perovskite films deposited on glass substrates to higher doses of radiation resulted in even more pronounced enhancement of the luminescence: 5- and 7-fold increases were observed by applying 2500 Gy and 5000 Gy, respectively (Fig. S5a, SI). It should be emphasized that the gamma rays-induced changes in the emission spectra were essentially reversible: repeating the measurements 2 weeks after radiation exposure revealed only three times stronger PL intensity for 5000 Gy exposed samples, while the red shift of the bands completely disappeared (Fig. S5b, SI). The observed PL dynamics is inconsistent with the expected radiation-induced defect (trap) formation mechanism, which should result in a severe quenching of the photoluminescence. However, the increase in the PL intensity and red-shift of the emission bands were both welldocumented for the mixed halide perovskite films exposed to light and are known in the literature as “Hoke effect”.25-27 We explored the PL dynamics of the triple-cation perovskite films under illumination with the green laser (532 nm). Indeed, the films demonstrated very


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characteristic behavior reflected in the gradual enhancement of the PL intensity while increasing the laser light exposure time from 30 s to 30 min. Finally, we observed three times more intense emission than for pristine films, while the maximum of the emission band shifted from 770 to 788 nm (Fig. 3b). The samples deposited on glass substrates demonstrated 10-fold increase in the PL intensity over 13 min of laser exposure and red-shifting of the emission band by 17 nm (Fig. S5c, SI).

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Figure 3. PL spectra of glass/ITO/PEDOT:PSS/perovskite films measured at least 1 h after exposure to gamma rays with the doses of 0-500 Gy (a) and green laser light (532 nm, 0.238 mW) (b) demonstrating the dynamics characteristic for the Hoke effect. PL spectra of the perovskite films exposed to white light illumination (100 mW/cm2, nitrogen atmosphere) revealing the photochemical degradation of the films accompanied with the quenching of the photoluminescence due to the trap formation (c). The relaxation of the light-induced changes was monitored while keeping the samples in the dark and measuring their PL spectra with a short (10 to ~6.0% and Jsc decreased from ~18 to ~11 mA/cm2 as also supported by EQE measurements (Fig. 4b, Figs. S12-S13, SI). The Jsc values extracted from J-V measurements were reconfirmed by the integration of the EQE spectra against the standard AM1.5G solar spectrum (Figs. S14 and S15, SI). Interestingly, FF and particularly VOC remained almost unaffected by gamma radiation for


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both types of samples, which indicates that the main degradation mechanism is not related to the trap formation. The appearance of the traps usually increases the density of states in the gap, which leads to the VOC losses.31,32 We strongly believe that the device degradation is mainly induced by the radiation-induced halide phase segregation similar to the Hoke effect. According to the previous reports, the light-induced phase segregation leads to the formation of recombination centers and causes reduction in the short circuit current density.25,28 Most probably, gamma rays-induced halide segregation causes similar effects.


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Figure

4.

PCE

and

Jsc

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functions

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dose

delivered

to

the

glass/ITO/PEDOT:PSS/perovskite (a) and glass/ITO/PEDOT:PSS/perovskite/PC61BM (b) samples.

Particularly interesting is the fact, that PC61BM does not stabilize the perovskite layer and, on the contrary, contributes to the overall degradation of the system. This observation suggests that PC61BM is intrinsically unstable with respect to the radiation exposure. To verify this hypothesis we exposed a bulk sample of PC61BM to a high dose of gamma rays (5000 Gy) and then applied it as electron transport material in the ITO/PEDOT:PSS/perovskite/PC61BM/Ag solar cells (note that PC61BM was the only device component exposed to radiation in that case). Fig. S16 (SI) shows that the solar cells comprising exposed PC61BM deliver notably lower current densities and power conversion efficiencies as compared to the reference devices fabricated using pristine PC61BM sample. The origin of the radiation-induced degradation of PC61BM remains unclear, though gamma rays induced polymerization, cage rupture and formation of radicals can be suspected according to the previously performed comprehensive studies of the radiation chemistry of fullerenes.33 To summarize, we investigated the impact of gamma radiation on the behavior of the complex lead halide Cs0.15MA0.10FA0.75Pb(Br0.17I0.83)3 perovskite solar cells in order to estimate the potential of such devices for space applications. It was shown that the doses up to 500 Gy do not damage the hole collecting bottom electrode glass/ITO/PEDOT:PSS. However, radiation affects significantly the photovoltaic performance of the perovskite absorber and the electron transport PC61BM layers. The main contribution to the solar cell degradation comes from the severe


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photocurrent losses (25-35% of the initial value) originating, most probably, from the halide phase segregation induced by high radiation doses, which we observed here for the first time. Therefore, the existing perovskite materials probably have insufficient radiation stability for considering their application into space technologies. However, rapid progress in the field of perovskite photovoltaics sooner or later will bring a new generation of absorber materials showing significantly improved radiation stability. These studies might provide impetus for developing scalable and high performance applications of perovskite solar cells in space missions.

Acknowledgements This work was supported by Russian Science Foundation (project No. 18-13-00353). The XPS measurements were supported by Russian Science Foundation (project 17-72-10044). Supporting Information Experimental procedures and figures S1-S16 showing characteristics of devices with exposed Glass/ITO/PEDOT:PSS layers and Glass/ITO/PEDOT:PSS/perovskite/PC61BM layers, UV-vis, XRD, XPS, PL, KPFM, and EQE data.

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Gamma Rays Induced Decomposition in the Triple-Cation Perovskite

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