Effect of Electron Transporting Layer on Bismuth-Based Lead-Free

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Effect of electron transporting layer on Bismuth based lead free perovskite (CH3NH3)3 Bi2I9 for photovoltaic applications Trilok Singh, Ashish Kulkarni, Masashi Ikegami, and Tsutomu Miyasaka ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.6b02843 • Publication Date (Web): 26 May 2016 Downloaded from http://pubs.acs.org on May 30, 2016

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ACS Applied Materials & Interfaces

Effect of electron transporting layer on Bismuth based lead free perovskite (CH3NH3)3 Bi2I9 for photovoltaic applications Trilok Singh ‡, *, Ashish Kulkarni ‡, Masashi Ikegami and Tsutomu Miyasaka* Graduate School of Engineering, Toin University of Yokohama, 1614 Kuroganecho, Aoba, Yokohama 225-8503, Japan ABSTRACT: Methylammonium iodo bismuthate ((CH3NH3)3Bi2I9) (MBI) perovskite is a promising alternative to rapidly progressing hybrid organic-inorganic lead perovskites due to its better stability and low toxicity compared to lead-based perovskites. Solution-processed perovskite fabricated by single-step spin-coating and subsequent heating produced polycrystalline films of hybrid perovskite (CH3NH3)3Bi2I9) whose morphology was influenced drastically by the nature of substrates. The optical measurements showed a strong absorption band around 500 nm. The devices made on anatase TiO2 mesoporous layer showed good performance with current density over 0.8 mA cm-2 while the devices on brookite TiO2 layer and planar (free of porous layer) was inefficient. However, all the MBI devices were stable to ambient conditions for more than 10 weeks. KEYWORDS: Lead free perovskite, Methylammonium iodo bismuthate (MBI), hybrid perovskite, TiO2 compact layer (CL), TiO2 anatase mesoporous, TiO2 brookite mesoporous, Stability.

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INTRODUCTION The generation of renewable energy is one of the vital issues of the present century and solar energy can be an important contributor to future energy production whereas the production of solar cells is rapidly increasing with comprehensive decrease in solar cells price. However, to compete with other energy generation sources in order to grow a large-scale energy source, the production cost of solar cells must be reduced further. Recently, the next generation solar cells employing hybrid organic–inorganic halide perovskites (ABX3 where A= organic cation, B= inorganic metal and X= halogen) as an active absorption layer have gained huge attention and established as a major field of research since the pioneering work from our group1,2. In a very short time, the research had already achieved a certified power conversion efficiency (PCE) of 21%, nearly approaching the performance of mature technologies3,4,5. The organic-inorganic perovskites possess excellent properties such as high absorption coefficient, tunable bandgap6,7, long carrier diffusion lengths8

,9 ,10

and

they can be produced by low cost solution

processes11,12,13,14,15. Despite the almost vertical growth in device performances still there are several issues to address. Apart from consistent fabrication processes and stability, the toxicity of lead (Pb) is presently a major disadvantage with the lead based perovskite solar cells. The primary challenge is to replace or reduce the amount of lead in the perovskite with a different and less toxic element. Recently, efforts have been made to replace toxic Pb with alternatives such as Sn,16,17,18,19 whereas its small bandgap can produce very high short-circuit current densities compared to the Pb-based perovskites. However, the device performance and open circuit voltage of Sn(II)-based perovskite has been limited by bulk recombination and in addition, the stability of Sn-based perovskite in ambient condition is very poor. Therefore, all the processes have to be carried out in the nitrogen gas atmosphere to avoid the degradation. The


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other perovskite materials without Pb also have been reported which showed low power conversion efficiency compared to the lead-halide perovskites, however, their stability is superior and also exhibit other functionalities20,21,22,23,24,25. Among these studied materials, methylalkylammonium iododibismuthate crystals (CH3NH3)Bi2I9, (MAIB or MBI) exhibited promising optoelectronic properties.26,27,28,29,30,31,32 However, their photovoltaic properties, reported recently by Park et al. where they have studied the photovoltaic characteristics of A3Bi2I9 perovskite and its suitability for two different cations (Cs and Methylammonium (MA)) with Cs3Bi2I9 , MA3Bi2I9 , and MA3Bi2I9Cl

x

materials using a single step spin coating, were

found to be very low.33 Lyu et al. have shown the promising stability of bismuth based perovskite on thick mesoporous configuration34. Further, Oez et al. studied an inverted cell of bismuth perovskite and observed the power conversion efficiency up to 0.1% with very high stability in ambient condition35. However, to the best of our knowledge, only few reports have shown the suitability of MBI perovskite in planar or mesoporous device structure whereas no comprehensive study on various device structures of MBI perovskite has been reported so far. Here, we report preparation of Bi-based halide perovskite (MBI) with the chemical formula (CH3NH3)3Bi2I9 in planar and mesoporous device structures via a simple, low-temperature solution process. A detailed morphological, structural and optoelectronic properties are studied for suitable device fabrication. We demonstrate a comparative study of perovskite formation on mesoporous (Anatase and Brookite TiO2) and planar structure and its strong dependence on the kind of TiO2 and device structure. Although the power conversion efficiency (PCE) is still low (0.2%), all the devices fabricated, irrespective of its structure, were stable for long time (5 weeks) under ambient air. Nevertheless, the results adequately evidence that morphology can play a significant role in improving cell efficiency of MBI perovskites. The development in low


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temperature processing of MBI can address both the toxicity and stability issues of lead-based perovskites. Experimental Section F-doped SnO2 (FTO) (10 Ω/□, NSG Group, Japan) conductive and transparent glass substrates were patterned using zinc powder and 3 M HCl aqueous solution and cleaned thoroughly with commercial detergent (2% Hellmanex in water), deionized water (DI), acetone and ethanol in a sonication bath sequentially, and thoroughly dried with nitrogen. All the chemicals in this study were used as received, without further purification. TiO2 Compact layer coating The TiO2 compact layer (CL) was spin-coated onto cleaned FTO glass by using 0.15 M titanium diisopropoxide bis-(acetylacetonate) (Ti acac) (75 wt% in isopropanol, Sigma-Aldrich) in a 2propanol (99.9%, Wako) solution at 3000 rpm for 30 seconds, followed by drying at 125°C for 5 minutes and cooled down to room temperature. Further two successive coatings (3000 rpm, 30 s) from 0.3 M Ti acac solution were carried out and dried at 125°C for 5 minutes. The spin coated FTO samples were further treated with 40 mM TiCl4 aqueous solution at 70°C for 60 minutes. The TiCl4 treated samples were thoroughly washed with DI water and dried in nitrogen. Then, these samples were annealed at 500°C for 30 minutes in a muffle furnace. TiO2 mesoporous coating An aqueous brookite TiO2 paste (PECC-B01, Peccell Technologies, Inc., particle size 10−20 nm) was diluted to 33 vol% with ethanol and spin-coated on the TiO2 compact layer at 3000 rpm for 30 s. The substrates were annealed at 300 °C for 1 h in a muffle furnace. The anatase


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mesoporous layer were spin-coated using a TiO2 paste (18NR-T, Dyesol, particle size ~20 nm) diluted in a 25 wt% ethanol at 4000 rpm for 30 s and the coated substrates were then sintered at 500 °C for 1 h in muffle furnace. The coated substrates (Planar and mesoporous) were treated with UV-Ozone for 10 minutes before the perovskite deposition. 20 wt% solution of bismuth triiodide (BiI3) and MAI in DMF were heated at 50°C for 30 minutes prior to the coating. The perovskite solution was spin coated on UV-ozone treated CL layer at 2000 rpm for 30 s. After spin coating, the samples were directly transferred to hot plate which was at 100°C and heated for 70- 90 min. The hole transporting material (HTM) was spin-coated (2000 rpm 30 s) from 8 wt% solution of spiro-OMeTAD in chlorobenzene solution containing additives of lithium bis(trifluoromethanesulfonyl) imide and 4-tert-butylpyridine. Then, the samples were kept overnight for ageing. Finally, Au metal electrode of 100 nm was thermally evaporated on top of the HTM to complete the device fabrication. Characterization The solar cell characteristics of all devices with an active area of 0.09 cm2 were measured with a Keithley 2400 source meter under 1 sun illumination (AM 1.5 G, 100 mW cm-2) using a Peccell Technologies PEC-L01 solar simulator. The EQE spectra of the devices were measured in air at room temperature with Peccell Technologies, PEC-S20 action spectrum measurement setup. The structural, optical and morphological analysis were carried out using X-ray diffractometer (D8 Discover, Brucker) with CuKα radiation source, UV-Vis spectrophotometer (UV-Vis 1800, Shimazdu) and scanning electron microscope (SU8000, HITACHI) respectively.


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Results and discussion


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Fig. 1 SEM top and cross section image of MBI perovskite layer deposited on (a-b) TiO2 compact layer (c-d) Brookite mesoporous and (e-f) Anatase mesoporous The top view SEM image of MBI films and cross-sectional view SEM images of different stacking layers of the perovskite devices of different architectures are displayed in Figure 1. Morphology of the MBI perovskite on planar differed slightly from that on mesoporous (brookite and anatase TiO2) substrates (Fig, a, c and e). Surface coverage of planar and anatase substrate with MBI was found to be similar and better than for brookite (Fig. 1b). It can be seen from cross-sectional SEM image that the HTM layer touches mesoporous layer in case of brookite mesoporous film. For planar and anatase case, the capping layer of MBI device resembles smooth interfaces. These results show how the surface properties of substrate affect the morphological properties of MBI perovskite layers dramatically.

Fig. 2 (a) XRD of MBI perovskite grown on Planar and mesoporous (Anatase and brookite) layer (#, FTO peaks) and (b) UV-vis of MBI perovskite (Inset of Fig 2b. shows the optical image of A=anatase, B=brookite and P= Planar).

Further, crystal structure of the MBI perovskite was determined from X-ray diffraction measurement, as shown in Figure 2 (a). The diffraction peaks well matched with the literature values, which were solved in the P63/mmc space group36. The diffraction peaks of MBI on all the


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three substrates showed close matching with each other except the intensity of the peak at lower angle (2 θ = 7.5) on planar CL was slightly higher than the other two. This enhancement in the intensity at lower angle can be attributed to the effect of scaffolds The optical absorption measurement showed the absorption band around 500 nm in all the samples and brookite samples had higher absorption due to greater thickness of the perovskite films. However, the optical images showed orange colour of all three samples (inset in Figure 2b).

Fig. 3 J-V curve of best performing MBI devices in both device architectures (Planar and mesoporous)

In order to study the influence of different substrates/morphology on the final photovoltaic performance, MBI perovskite solar cells (PSCs) with all three configurations (planar, mesoporous brookite and anatase TiO2) have been prepared following same experimental


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procedure. In Fig. 3, the current density (J)-voltage (V) characteristics of all the three solar cells, measured under standard conditions, are compared. The EQE spectra of all devices (Figure S1) showed an edge of the EQE spectra is around 620 nm, indicating same spectral responsivity of MBI and the integrated photocurrent density from EQE is well matched with the value obtained from standard illumination at 1 SUN. As can be seen in Fig. 3, PSCs prepared on anatase TiO2 mesoporous layer showed better photovoltaic performance in comparison to planar and brookite mesoporous PSCs. PSCs of brookite-based and planar structures resulted poor characteristics in all parameters of short circuit photocurrent, open circuit voltage, and fill factor. This indicates that these cells undergo high internal resistance and/or large recombination. Because carrier transfer resistance is directly influenced by junction structure between scaffold and MBI, it is rationalized that physical junction was poorly formed in case of brookite and planar scaffolds. The higher photocurrent of anatase TiO2 MBI cells can also be attributed to better surface coverage (Table S1). These results demonstrate that MBI perovskites for solar cell applications depends strongly on the compact layer and kind of scaffold employed. As can be seen, PSCs prepared on anatase TiO2 mesoporous layer showed better results in terms of efficiency, open circuit voltage and short circuit current in comparison to planar and brookite mesoporous PSCs. An important correlation between various solar cell parameters (Fig. 4) of all studied device architectures has been observed. Planar and brookite MBI samples formed the non-uniform perovskite films, as evident from the cross-sectional SEM images (Fig. 1 b and 1 d), which lead to the increased shunting pathway because of contact between spiro-OMeTAD and TiO2 compact layer (brookite-mesoporous). addition, we have seen that the perovskite loading is very poor in case of thicker brookite mesoporous layer which is in contrary to the lead based perovskite and this poor loading of MBI


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in brookite mesoporous can be attributed to the strong inter particle necking of brookite leading to

Fig. 4 Device performance at optimized conditions using different device architectures measured under simulated AM 1.5 sunlight of 100 mWcm2 irradiance. The data are represented as a standard box plot with (a) Short circuit current density (Jsc), (b) open circuit voltage (Voc), (c) Fill factor (FF) and (d) Efficiency (η).

smaller pores and fast crystallization of MBI37,38,39 In contrast, in case of anatase MBI device, being rich of pores, the film coverage is good and interfaces of various layer are smooth compared to planar and brookite. The continuous interfaces in anatase mesoporous TiO2-


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perovskite reduces junction resistance as well as charge recombination and produces higher Voc as well as better Jsc. Recently, Lyu et al. have shown that the carrier density of the MBI is ~1016 cm-3, which is 7 orders of magnitude higher than MAPbI3 (109 cm-3)40. Such high background carrier densities in the light-absorber can contribute to the bulk recombination which further influence and reduce the FFs. The other factors that can drastically change the device performances are the presence of defects and impurities in MBI. However, we observe no additional absorption band in UV-Vis

(Fig. 2 b) spectra and also no impurity phases in XRD. In the present study, the MBI perovskite showed almost no hysteresis in all the device configurations (Figure S2). The long term stability of best performing devices showed good PCE after 10 weeks, the devices were kept in ambient conditions after each measurements without any sealing (Fig.5).


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Fig. 5. Long term stability of MBI perovskite in ambient conditions and the device also stored in ambient.

Based on our results obtained for the influence of TiO2 electron collectors, the most important issue to enhance the Bi-based cell performance must be structuring of continuous interfaces at collector-perovskite hetero-junction and suppression of recombination at the interfaces including the grain-grain inter-structure of perovskite crystals. With spectral sensitivity for photon collection (< 620 nm), we estimate that MBI perovskite as potential to yield Jsc as high as 10 mA cm-2. The corresponding efficiency level with Voc of 1 V is around ~ 8%. The carrier diffusion length will also limit the thickness of the MBI absorber. Assuming 100 nm thick MBI perovskite film, efficiency is limited < 4%. Present study shows that there are large room for improvements in the quality of MBI perovskite absorber via controlling the nucleation and growth of MBI crystals and appropriate choice of substrates as the degree of lattice mismatching will also play a pivotal role in preferential growth and nucleation. Here, controlling the I/Bi stoichiometry is essential in the crystallization process. Optoelectronic properties (light absorption coefficient) are also very sensitive to the stoichiometry of organic halide and choice of salts as the final film is not only sensitive to experimental conditions (stoichiometry, solvent, heating etc.), but can be predetermined via desired/undesired colloids in the precursor solutions. These improvements will lead to minimise recombination and enhance the photovoltaic parameters of the bismuth based organic-inorganic materials. Further optimization of the growth conditions and preparations is required to exploit maximum potential of MBI.

Conclusions


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In summary, we have shown facile synthesis of MBI perovskite at low temperature via single step spin coating of stoichiometric solution of bismuth tri iodide and methylammonium iodide in DMF. The suitable device configuration of MBI perovskite using planar, brookite and anatase mesoporous layer for efficient perovskite photovoltaic have been investigated. The morphology of MBI depended strongly on the compact and mesoporous layer on the FTO substrates. MBI growth on planar substrates is not continuous which further facilitate the non-uniform growth, however, in case of mesoporous layers the nucleation and growth is more uniform. In case of brookite, the inter particle necking impedes the MBI percolation in the pores and hampers the nucleation and uniform growth of MBI. The photovoltaic analysis showed improved performance with 0.2% PCE with good stability of device for 10 weeks in ambient condition. Furthermore, the presented study showed that the MBI perovskite has immerged as a very promising material for use in optoelectronic devices particularly in hybrid solar cells. ASSOCIATED CONTENT Supporting Information. Histogram plot of different cases studied here, EQE spectra and photocurrent-density (J)-voltage (V) curve, this material is available free of charge via the …. AUTHOR INFORMATION Corresponding Authors *[email protected] and [email protected] Present Addresses † Graduate School of Engineering, Toin University of Yokohama, 1614 Kuroganecho, Aoba, Yokohama 225-8503, Japan


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Author Contributions ‡ Contributed equally to this work The manuscript was written through contributions of all authors. All authors have given approval to the final version of the manuscript.

ACKNOWLEDGMENTS TS would like to acknowledge the Japan Society for the Promotion of Science (JSPS) for the JSPS postdoctoral fellowship. This study was supported by Japan Science and Technology Agency (JST), Advanced Low Carbon Technology R&D program (ALCA). TM acknowledge financial support from Japanese Society for Promotion of Science (JSPS) Grant-in-Aid for Scientific Research B Grant Number 26289265. We thank Prof. Hiroshi Segawa for allowing access to research facilities at Research Center for Advanced Science and Technology (RCAST), University of Tokyo. We thank to Ajay Jena for valuable discussion and helping in SEM.

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39 Kogo, A.; Sanehira, Y.; Ikegami, M.; Miyasaka, T, Anatase and Brookite Electron Collectors from Binder-free Precursor Pastes for Low Temperature Solution-processed Perovskite Solar Cells, Chem. Lett, 2016, 45, 143-145. 40 Stoumpos, C., C.; Malliakas, C., D.; Kanatzidis, M., G. Semiconducting Tin and Lead Iodide Perovskites with Organic Cations: Phase Transitions, High Mobilities, and NearInfrared Photoluminescent Properties. Inorg. Chem., 2013, 52, 9019-9038.


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TOC graphic 337x181mm (150 x 150 DPI)


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Effect of Electron Transporting Layer on Bismuth-Based Lead-Free

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