Rear surface passivation by melaminium iodide additive for stable and

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Rear surface passivation by melaminium iodide additive for stable and hysteresis-less perovskite solar cells Seul-Gi Kim, Jiangzhao Chen, Ja-Young Seo, Dong-Ho Kang, and Nam-Gyu Park ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.8b06616 • Publication Date (Web): 11 Jul 2018 Downloaded from http://pubs.acs.org on July 11, 2018

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ACS Applied Materials & Interfaces

Rear surface passivation by melaminium iodide additive for stable and hysteresis-less perovskite solar cells Seul-Gi Kim,† Jiangzhao Chen,† Ja-Young Seo, Dong-Ho Kang and Nam-Gyu Park* School of Chemical Engineering, Sungkyunkwan University (SKKU), Suwon 440-746, Korea

†

These authors equally contributed to this work

*Corresponding author E-mail: [email protected], Tel: +82-31-290-7241

Abstract Surface passivation of perovskite grains is one of promising methods to reduce recombination and improve stability of perovskite solar cell (PSC). We report here effect of melaminium iodide additive on photovoltaic performance of PSC based on (FAPbI3)0.875(CsPbBr3)0.125 perovskite. Cyclic –C=N- and primary amine in melamine are good hydrogen bond acceptor and Lewis base, which can interact with both organic cation and Lewis acidic lead iodide in perovskite film. Melaminium iodide is synthesized and added in the precursor solution, which is directly spin-coated to form the perovskite film. The presence of melaminium iodide additive reduces trap density from 1.02 × 1016 cm-3 to 0.645 × 1016 cm-3, which leads to reducing non-radiative recombination and thereby improving mean open-circuit voltage and fill factor from 1.054 V to 1.095 V and from 0.693 to 0.725, receptively. In addition, photocurrent-voltage hysteresis is reduced by the melaminium iodide additive, which results in enhancing average power conversion efficiency (PCE), obtained from reverse and forward scanned data, from 15.86% to 17.32%. Time-resolved photoluminescence confirms that melaminium iodide plays more important role in passivating rear surface of perovskite layer contacting hole transporting spiro-MeOTAD layer. Aging test under relative humidity of 65% 1

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revels that melaminium iodide improves stability because of suppression of defect evolved by moisture. Keywords: perovskite solar cell; passivation; melamine; melaminium iodide; hysteresis; stability; preferred orientation

Introduction Perovskite solar cell (PSC) based on organic-inorganic lead halide perovskite has been regarded as a disruptive technology in photovoltaics thanks to its superb photovoltaic performance better than high efficiency thin film solar cells. Research activity on PSC was triggered by the reports on high efficiency, stable solid-state perovskite solar cells in 2012,1, 2 following the less-attentive but important reports on perovskite-sensitized solar cells in 20093 and 2011.4 The initial power conversion efficiency (PCE) of about 10% in 2012 rose unprecedentedly and sharply to 22.7% in 2017 and the PCE of PSC now surpasses those of the conventional and commercially available solar cells based on CIGS (22.6%), CdTe (22.1%) and poly Si (22.3%).5 Although PSC demonstrated very high PCE, current-voltage (I-V) hysteresis and stability have been issued to be solved for commercialization. I-V hysteresis phenomenon, mismatch of I-V curves between scan directions, was first issued by Snaith et al. in 2014.6 Regarding origin of the hysteresis, several factors affecting the scandependent I-V curves have been explored such as ferroelectric behavior,7 accumulation of charges at interfaces8,9 native defects of perovskite,10,11 dynamic motion of organic cations12,13 and ion migration.14,15 Since stability of the device with pronounced hysteresis was reported to be poorer than that of the hysteresis-less device,16,17 reduction and/or removal of the hysteresis is important. Defects due to missing halide anion and/or organic cation at grain boundaries in polycrystalline perovskite can act as centers for non-radiative recombination, which is unfavorable for the performance and might cause the hysteresis as well.18,19 The under-coordinated Pb atoms due to missing iodide, can also act as electronic trap states20 which could be passivated by electron-donating Lewis bases such as thiophene or pyridine.21 This indicates that interfacial engineering is of importance in order to passivate surface or grain boundary of perovskite film and thereby to improve PCE and stability.22−28 In 2


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the last few years, it was reported that the presence of Cs and Br in FAPbI3, leading to mixed cation and anion, could improve PCE and reduced hysteresis due to improved crystallinity and decreased defect density.29,30 Nevertheless, on the contrary to the reports, many of these PSCs still show the hysteresis.31 Melamine is an organic base and a trimer of cyanamide with a 1, 3, 5-triazine skeleton, which has been widely used for food additive, fire retardant, metabolite and so on. We are motivated to use melaminium iodide as a defect passivation material in FA base mixed PSC because it has dual function of Lewis base and strong hydrogen bond acceptor, which is expected to control the

hysteresis.

Here,

we

report effect of melaminium

iodide in

the

(FAPbI3)0.875(CsPbBr3)0.125 perovskite layer on photovoltaic performance and stability. Melaminium iodide additive is directly added to the precursor solution. Ultraviolet spectroscopy (UPS) is measured to study change of band alignment after introduction of melaminium iodide. Photovoltaic parameter and I-V hysteresis are compared before and after introduction of melaminium iodide. Time-resolved photoluminescence (TRPL), Urbach tail energy and trap density are measured to explain the basis for the reduced hysteresis and the enhanced photovoltaic parameters after introduction of melamine. Moisture-stability is investigated under relative humidity of 65% in the dark to compare effect of melaminium iodide additive.

Results and discussion Figure 1 (a) shows chemical structure of melamine based on 1,3,5-triazine. Since melamine is Lewis base because of three primary amines, it can interact with Lewis acid like PbI2.32 In addition, as can be seen in Figure 1(a), nitrogen in cyclic carbon-nitrogen (-C=N-) bond can act as a hydrogen bond acceptor.33−35 The bi-functionality of Lewis base and hydrogen bond acceptor is expected to interact with Lewis acid and organic cation in organic-inorganic halide perovskite.36−39 In order to investigate effect of melaminium iodide additive on photovoltaic performance, there are two ways via either post-treatment or direct mixing in the precursor solution. Since melaminium iodide is less soluble in IPA for the post-tretaement, melaminium iodide was directly mixed in perovskite precursor solution. As a mother composition, we select (FAPbI3)0.875(CsPbBr3)0.125 (FAPbI3)0.875(CsPbI3)0.125 perovskite films 3



without and with melaminium iodide are formed by an adduct approach according to the method reported elsewhere.36 Figure 1 (b) shows photographs of PSCs and precursor solutions with different concentration of melaminium iodide (the ratio of melaminium iodide to lead ion [melaminium iodide]/[Pb2+] is designated as [M]/[Pb] = x and x ranges from 0 to 0.015). Precursor solutions turn dark yellow as concentration of melaminium iodide increases, which might result from interaction of precursor ions with melaminium iodide. In addition, PSCs show that the color after spin-coating spiro-MeOTAD changes from green to red, which is likely to be due to modification of grain surface by melaminium iodide additive. In Figure 1(c), coating process is schematically illustrated, where melaminium iodide is added in the perovskite precursor solution and then it is spin-coated on the substrate. While spinning, diethyl ether is dropped to induce Lewis acid-base adduct as an intermediate phase prior to form perovskite film.36 Melaminium iodide cannot be included in 3D perovskite lattice because of its larger ionic radius, which means it tends to be located on the surface of perovskite grains. When considering the thermal annealing process, there will be temperature gradient between top and bottom of the perovskite film because bottom of the perovskite film is relatively in direct contact with thermal heater, while temperature will decrease from bottom to top in the film because of air/solid interface. Thus, perovskite is expected to grow from the bottom of the perovskite adduct layer, which is expected to push melaminium iodide to the rear surface of the perovskite film.

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Figure 1. (a) The chemical structures of melamine. (b) Photographs of (FAPbI3)0.875(CsPbBr3)0.125 perovskite solar cells. Inset shows the precursor solution without (x = 0) and with melaminium iodide (0.002599.5%, Sigma Aldrich). Melaminium iodide stock solution in DMF was prepared by dissolving 0.0254g of melaminium iodide in 1 mL of DMF. For [Melamine]/[Pb] = 0.010, 0.1 mL of pure DMF was replaced by the stock solution to the perovskite precursor solution., 0.025 mL – 0.15 mL of melaminium iodide stock solution was mixed with the perovskite precursor solution to prepare [Melamine]/[Pb] = 0.0025, 0.0050, 0.0075, 0.01, 0.0125, 0.015 of melaminium solutions. The total DMF volume was set 0.57 mL. The solutions were filtered with PTFE filter (0.45 µm pore size, Whatman). The 25 µL of precursor solution with and without melaminium iodide was spin-coated on the top of mTiO2 layer at 4000 rpm for 20 s, where 0.3 mL of diethyl ether (≥99.7%, anhydrous, SigmaAldrich) was dropped while spinning to induce intermediate adduct film. The perovskite layers were formed by annealing at 140 oC for 15 min. The 20 µL of spiro-MeOTAD [2,2′,7,7′-tetrakis-(N,N-di-4-methoxyphenylamino)-9,9′-spirobifluorene] solution, containing 72.3 mg spiro-MeOTAD, 28.8 µL of 4-tert-butyl pyridine and 17.5 µL of lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) solution (520 mg LiTSFI in 1 mL acetonitrile (99.8%, Sigma Aldrich)) in 1 mL of chlorobenzen, was spin-coated on the perovskite layer at 3000 rpm for 30 s. Finally, Au electrode was deposited by thermal evaporation at a constant evaporation rate of 0.3 Å/s for 80 min. Characterizations Photocurrent density (J)-voltage (V) curves were measured under AM 1.5G one sun (100 mW/cm2) illumination using a solar simulator (Oriel Sol 3A, class AAA) equipped with 450 W Xenon lamp (Newport 6280NS) and Kiethley 2400 source meter. The light intensity was adjusted by NREL calibrated Si solar cell having KG-5 filter. The device was covered with a metal mask with aperture area of 0.125 cm2 during the measurement. X-ray diffraction (XRD) patterns were obtained using a D8 Advance (Turbo X-Ray Source, 18 KW, Bruker 24


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Corporation) under Cu-Kα radiation (λ = 1.5406 Å). Perovskite film morphology was investigated by means of a scanning electron microscope (SEM, JSM-7600F, JEOL). Absorption spectra were measured using an UV-Vis spectrometer (Lambda 45, Perkin Elmer). Urbach tail energy (Eu) was estimated by α = αo exp (hν/Eu),50,51 where α is absorption coefficient and αo is a constant. Electrochemical impedance spectroscopy (EIS) measurements were performed under 0.85 sun illumination (85 mW/cm2) in the dark using PGSTAT 128N (Autolab, Eco-Chemie). DC voltage was applied from 0 V to 0.4 V for the device with FTO/(FAPbI3)0.875(CsPbBr3)0.125/Au layout or 1 V for the device with FTO/TiO2/(FAPbI3)0.875(CsPbBr3)0.125/spiro-MeOTAD/Au layout at 0.1 V intervals with small perturbation of AC 20 mV sinusoidal signal. Frequency ranged from 0.1 Hz to 10 kHz. Trap density was estimated by using SCLC (Space-Charge-Limited Current) method. Devices with the FTO/perovskite/Au structure were measured in the dark from 0 V to 1.0 V with the scan rate of 1000 ms. The observed response was analyzed according to SCLC theory. Trap density (nt) was estimated using the relation VTFL = entd2/2εε0,54−56 where VTFL is the trapfilled-limited voltage, e is electric charge (1.602 × 10-19 C), ε is dielectric constant, ε0 is the vacuum permittivity (8.8542 × 10-14 F/cm) and d is film thickness. The dielectric constant was calculated using the equation of ε = Cd/Aε0, where C is geometrical capacitance at high frequency (~10-4 Hz).57,58 Steady-state photoluminescence (PL) and time-resolved PL (TRPL) were measured by a Quantaurus-Tau compact fluorescence lifetime spectrometer (Quantaurus-Tau C11367-12, Hamamatsu). The film samples were excited with 464 nm laser (PLP-10, model M12488-33, peak power of 231 mW and pulse duration of 53 ps, Hamamatsu) pulsed at repetition frequency of 10 MHz for steady-state PL and 500 kHz for TRPL. External quantum efficiency (EQE) was measured by a EQE system (PV measurement Inc.), in which a monochromatic beam was generated from a 75 W Xenon source lamp (USHIO, Japan). EQE data were collected in the DC mode without light bias. Ultraviolet photoelectron spectroscopy (UPS) measurements were carried out on ESCALAB 250 XPS system (Thermo Fisher Scientific) with HeI (21.2 eV). ATR-FTIR spectral data were collected using Bruker IFS-66/S (TENSOR27).

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AUTHOR INFORMATION Corresponding Author *E-mail (N.-G. Park): [email protected]. Tel: +82-31-290-7241.

ORCID Nam-Gyu Park: 0000-0003-2368-6300

Author Contributions N.-G.P., S.-G.K. and J.C conceived of the concept. N.-G.P. and S.-G.K. conceived experiments, performed data analysis, and prepared the manuscript. J.-Y.S performed and analyzed Impedance spectroscopy. D.-H.K characterized J-V curve and analyzed. All authors discussed the results and commented on the manuscript.

Acknowledgements This work was supported by the National Research Foundation of Korea (NRF) grants funded by the Ministry of Science, ICT Future Planning (MSIP) of Korea under contracts NRF2012M3A6A7054861 and NRF-2014M3A6A7060583 (Global Frontier R&D Program on Center for Multiscale Energy System) and NRF-2016M3D1A1027663 and NRF2016M3D1A1027664 (Future Materials Discovery Program). This work was also supported by Basic Science Research Program through the NRF under contact 2016R1A2B3008845 and NRF-2017H1A2A1046990 (NRF-2017-Fostering Core Leaders of the Future Basic Science Program/Global Ph.D. Fellowship Program).

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Rear surface passivation by melaminium iodide additive for stable and

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