Design and Synthesis of 1D-Polymeric Chain Based [(CH3NH3

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Design and Synthesis of 1D-Polymeric Chain Based [(CH3NH3)3Bi2Cl9]n Perovskite: A New Light Absorber Material for Lead Free Perovskite Solar Cells Khursheed Ahmad, Shagufi Naz Ansari, Kaushik Natarajan, and Shaikh M. Mobin ACS Appl. Energy Mater., Just Accepted Manuscript • DOI: 10.1021/acsaem.8b00437 • Publication Date (Web): 24 May 2018 Downloaded from http://pubs.acs.org on May 27, 2018

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ACS Applied Energy Materials

Design and Synthesis of 1D-Polymeric Chain Based [(CH3NH3)3Bi2Cl9]n Perovskite: A New Light Absorber Material for Lead Free Perovskite Solar Cells Khursheed Ahmad,a Shagufi Naz Ansari,a Kaushik Natarajanc and Shaikh M. Mobin*a,b,c a

Discipline of Chemistry, bDiscipline of Biosciences and Bio-Medical Engineering and cDiscipline of Metallurgy Engineering and Materials Science, Indian Institute of Technology Indore, Simrol, Khandwa Road, Indore 453552, India.

560cd/m2.14 This suggests that CH3NH3PbX3 possess multifunctional properties and could be employed in various applications. Although, CH3NH3PbX3 perovskites are desired material for various applications but the low stability, high sensitivity towards water, moisture and the presence of highly toxic lead (Pb) restrict their commercialization.15 Therefore, recently efforts have been made to improve the stability of the CH3NH3PbX3 perovskites. Masi et al. grow the perovskites in to the polymers to improve the stability but this fabricated device showed the poor PCE of 3%.16 Yao et al. introduced polymeric-ammonium cation and the PCE was reached to 8.7%.17 Further, Zuo et al. and Jiang et al. have prepared the polymer decorated MAPbI3 perovskite with enhanced PCE of 18.8% and 19.19%, respectively with improved moisture stability.18,19 However, the presence of Pb still remains a great challenge for the environment. This prompted us to design and find out a highly stable and Pb free perovskite materials for optoelectronic applications.

ABSTRACT: Although traditional perovskite solar cells have made tremendous progress in terms of efficiency but presence of toxic lead restricted their commercialization. Herein, we report first example of facile synthesis and newly designed highly stable lead-free methyl ammonium bismuth chloride in the form of 1Dpolymeric chain based perovskite. The formation of 1D-polymeric chain with formula, [(CH3NH3)3Bi2Cl9]n (1), has been authenticated by its single crystal X-ray diffraction (SCXRD) studies. The lead free 1 has been employed as an alternative to the traditional CH3NH3PbX3 perovskite with an excellent open circuit voltage of 430mV. KEYWORD: [(CH3NH3)3Bi2Cl9]n 1D-polymer, lead free perovskite, light absorber, photovoltaic, open circuit voltage and high moisture tolerance. Metal-organic hybrid perovskites with a general formula of AMX3 (A= organic group; M= metal ion and X= halide ions) has emerged as a rising star in the field of optoelectronic or photovoltaic applications.1-7 The CH3NH3PbX3 (X=halogen ions) perovskite have been the breakthrough in the field of perovskite solar cells and in the year of 2017, the power conversion efficiency of the lead based perovskite solar cells has been boosted to 22.1%.8 The use of CH3NH3PbX3 perovskites was not limited to solar cells but also employed in other applications because of their excellent features like higher absorption coefficient, tunable band gap, excellent conductivity and high carrier mobility.2-6 Liang et al. has developed the photo-detector by decorating the CH3NH3PbI3 perovskite with reduced graphene oxide.9 Later Dai et al. and Nuria et al have introduced the CH3NH3PbX3 perovskites in the construction of anode for battery applications and achieved the excellent results with stable specific capacity of 200 mAhg−1.10-11 More recently, Ogale and co-workers developed a novel anode for alkali-ion batteries which has shown good capacity of 646 mAhg−1 at 100 mAg-1 and stability up to 250 cycles.12 Moreover, Wang et al. used a novel strategy to develop the high performance supercapacitors.13 They have connected the perovskite solar cells with polymer based supercapacitor and the extremely high open voltage of 1.45 V was obtained. Yabing et al. used the chemical vapour deposition method to prepare the CH3NH3PbBr3 perovskite with surface roughness below 10 nm for the construction of the light emitting diode which showed the good luminance of

Bismuth (Bi3+) ion shows the similar isoelectronic behaviour to that of Pb2+ in the ionic radii and electronegativities.20,21 Moreover, the low toxicity and less explored bismuth opens new door for the researchers to synthesize the bismuth based perovskites. Herein, we report design and synthesis of a one dimensional (1D) polymeric chain of methyl ammonium bismuth chloride perovskite. In a simple synthetic strategic route, the 1D-polymeric chain of [(CH3NH3)3Bi2Cl9]n (1) was prepared by slow diffusion of the methanolic solution of BiCl3 into aqueous solution of CH3NH3Cl at room temperature (Scheme 1).

Scheme 1. Schematic representation showing synthetic route of 1. 1 was further authenticated by single crystal x-ray diffraction (SCXRD) studies. Moreover, the proposed combination of the

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fabricated lead free perovskite solar cells with a novel device architecture (ITO/BL-TiO2/Meso-TiO2/[(CH3NH3)3Bi2Cl9]n/SpiroMeOTAD/Au) was employed. The fabricated PSCs device showed the excellent open circuit voltage of 430 mV.

(red) obtained from SCXRD. Moreover, the 1 was exposed to the air for 2h (conditions; humidity:40%, temperature:30°C) and found to be highly stable in nature as confirmed by the PXRD patterns which shows no significant changes (Figure 2B). The optical behavior of the 1 was examined by the UV-vis absorption spectrum which showed a broad absorption peak between 400-500 nm (Figure 2C) and the band gap was calculated to be 2.85 eV by using Tauc relation (Figure 2D).

On contrary to earlier reports, where [(CH3NH3)3Bi2Cl9]n was prepared by using an excess of concentrated HCl,22 the single crystals of [(CH3NH3)3Bi2Cl9]n (1) were grown at room temperature by simple layering method without using any acids. 1 crystallizes in centrosymmetric orthorhombic, Pnma space group (Table S1). In crystal structure Bi atoms are coordinated by three terminal Cl atoms and three bridging Cl atoms which extend to form a 1D polymeric chain in two different fashions both aligned along b-axes (Figure 1a). In the unit cell, the complex anion contains two alternate face-sharing octahedra with two bridging Cl atoms (Figure 1b).

Figure 2. Characterization of 1: (A,B) PXRD, (C) UV-vis absorption spectrum and (D) Tauc plot. Further, the x-ray diffraction pattern for the prepared 1-film on ITO glass substrate in the 2θ range of 5-60° shows highly crystalline nature and phase purity (Figure 3A). The crystallite size of the 1-film was calculated to be 133.9 nm. The PXRD of the 1-film shows only diffraction peak in the highly oriented direction whereas the PXRD of 1 powder shows many peaks from the other crystal planes.20

Figure 1. Crystal structure of 1: a) Perspective views of 1Dpolymeric chain b) Positions of 1 and methylamine anion (CH3NH3) in the unit cell c) Distorted Octahedral geometry of Bi ions in Bi2Cl63─ anion. (Hydrogens are omitted for clarity) and (d) stacking in polymer 1. As shown in Figure 1, In 1, the Bi-ions are deviated from the center of the octahedron formed by the six chloride ions this may be due to the repulsion of Bi3+ ions. The Bi…Bi distances were found to be 5.693 Å and 5.672 Å. This repulsion among Bi3+ ions consequences in the movement of Bi-ions away from the shared octahedral face which results in a slight deviance from octahedral angles, Cl6–Bi1–Cl3 (91.16 Å) and Cl1–Bi1–Cl2 angle (93.30 Å) (Figure 1c), (Table S2). Terminal Bi−Cl bond distances are in the range of 2.572(10) Å which significantly shorter than the bridging Bi−Cl bonds of 2.835(10) Å, (Table S3). However, resulting electronic dipole moments is non-zero unlike (CH3NH3)Bi2I9 where electronic dipole within each dimer points in opposite directions giving a net zero dipole moment.23-24 Stackings can be seen in the structure of 1 (Figure 1d), Intra-anionic Cl…Cl distances 5.558 Å, 5.482 Å in [(CH3NH3)3Bi2Cl9]n can be a base to deliver potential charge transport path. Furthermore, the PXRD pattern (black) in the 2θ range of 5-80° showed the highly crystalline nature (Figure 2A) and found to be in agreement with the simulated PXRD pattern

Figure 3. Characterization of [(CH3NH3)3Bi2Cl9]n 1D polymer film on ITO substrate; PXRD (A,B), FE-SEM (C) and JV characteristics of ITO/BL-TiO2/MesoTiO2/[(CH3NH3)3Bi2Cl9]n/Spiro-MeOTAD/Au device (D).

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ACS Applied Energy Materials In order to check the moisture tolerance of 1-film, the 1film was exposed to the air for 2h (conditions; humidity:40%, temperature:30°C). The PXRD patterns for the unexposed (black) and exposed (red) to air of the 1-film revealed no degradation or any additional peak of impurity which suggest that the 1-film is stable under atmospheric conditions (Figure 3B). Since, the film morphology and the quality play a crucial role in the performance of the devices of photovoltaic application, the FE-SEM images for the prepared 1-film were recorded which showed the uniform morphology of 1-film (Figure 3C) over whole surface area of ITO glass (Figure S2) and may be employed for the perovskite solar cell applications. The EDX spectrum 1-film showed the presence of C, N, Bi and Cl (Figure S1). The thickness of 1-film was found to be ~ 532nm (Figure S3) measured by spectroscopic ellipsometry analysis. The interesting band gap, robust 1D-polymeric nature and high stability of 1 prompted us to explore the photovoltaic applications. Thus, 1 was explored as a light absorber in the fabrication of lead free perovskite solar cells with a novel architectures of ITO/Meso-TiO2/[(CH3NH3)3Bi2Cl9]n/SpiroMeOTAD/Au (in absence of blocking layer) and ITO/BLTiO2/Meso-TiO2/[(CH3NH3)3Bi2Cl9]n/Spiro-MeOTAD/Au (in presence of blocking layer) as shown in Scheme 2 (a) and (b) respectively.

der similar conditions. The recorded J-V characteristic for the TiO2 blocking layer is presented in Figure S4 and the open circuit voltage of 317mV was obtained. This shows that the introduction of TiO2 blocking layer reduced the recombination rate and enhanced the open circuit voltage. In order to elucidate more details about the recombination lifetimes of the device with and without the blocking layer of TiO2, we utilised an electrochemical impedance spectroscopy (EIS) based method with close accuracy to thermal photo voltage or PL methods, initially proposed by Kumar et al.25 and adapted for use in our specific scenario. The equivalent circuit comprises of one series resistance and three RC elements in series. The equivalent circuit diagram and Nyquist plot is shown in (Figure S5), where the three RC series elements correspond to resistive and capacitive contributions from ITO interface (R1, C1), bulk contributions (R2, C2) corresponding to the material, and interface with the perovskite layer (R3, C3) with the corresponding time constants τ1, τ2 and τ3, whose values are listed in (Table S4) after fitting the electrochemical model described in inset of Figure S5. The material/bulk recombination lifetime is found to be around ~1400 ns, which is in the higher region for perovskite based materials in contemporary literature.26 The effective recombination lifetime τ2 increases from 1436 ns without the blocking layer to 1470 ns with the blocking layer, which is indicative of suppression of recombination due to the presence of the blocking layer. Furthermore, the interfacial recombination lifetimes also see an increase with presence of the blocking layer, thus confirming enhanced carrier transport properties imparted by the blocking layer. The values of the bulk/material recombination lifetime are very much comparable to values obtained in contemporary literature. Additionally, we have recorded the photoluminescence (PL) spectra for ITO/BL-TiO2/MesoTiO2/[(CH3NH3)3Bi2Cl9]n/Spiro-MeOTAD (red) and ITO/Meso-TiO2/[(CH3NH3)3Bi2Cl9]n/Spiro-MeOTAD (black). The obtained results are presented in Figure S6. The PL intensity for the ITO/BL-TiO2/MesoTiO2/[(CH3NH3)3Bi2Cl9]n/Spiro-MeOTAD (red) was noticeably reduced as compared to the ITO/MesoTiO2/[(CH3NH3)3Bi2Cl9]n/Spiro-MeOTAD (black) (Figure S6). Since PL intensity is related to the radiative recombination processes (1), the decrease in intensity indicates that the presence of blocking layer has reduced the recombination rate.27 The working mechanism of PSCs device is illustrated in scheme 2. The energy levels shown in scheme 2 have been taken from the reported literature and the HOMO and LUMO levels were calculated using the cyclic voltammetry (Figure S7) according to the previous report.28 The equations used for the calculation of HOMO and LUMO are given below;25 E (HOMO)= -e [Eox onset + 4.4] ………… (1) E (LUMO)= -e [Ered onset + 4.4] .………… (2)

Scheme 2. Schematic diagram showing the working mechanism of PSCs devices with (a) without blocking layer: ITO/Meso-TiO2/[(CH3NH3)3Bi2Cl9]n/Spiro-MeOTAD/Au and (b) with blocking layer: ITO/BL-TiO2/MesoTiO2/[(CH3NH3)3Bi2Cl9]n/Spiro-MeOTAD/Au architectures. The energy levels were taken from the reported literature. The probable HOMO and LUMO for 1 was predicted by using cyclic voltammetry. The performance of this Pb-free fabricated novel (ITO/BL-TiO2/Meso-TiO2/[(CH3NH3)3Bi2Cl9]n/SpiroMeOTAD/Au) was scrutinized by using J-V under the sunlight conditions (intensity of 1.5AM (100 mW/cm2). The recorded J-V characteristic for the above fabricated architecture is shown in Figure 3D. Although, the fabricated device showed poor power conversion efficiency (0.001%) with the current density in nano-amperes, but an excellent open circuit voltage of 430mV was obtained. This high open circuit voltage may be due to low recombination rate and the polymeric structure of 1 which rapidly injected the excited electrons to the conduction band of mesoporous TiO2 which transferred to the anode through blocking layer of TiO2. The presence of TiO2 blocking layer suppresses the chance of the injected electron to recombine either with 1 or spiroMeOTAD and resulted in the high open circuit voltage. To confirm that the TiO2 blocking layer reduces the recombination rate, we have fabricated the PSCs device in absence of TiO2 blocking layer and its performance was determined un-

Although, the performance of the light absorbers/PSCs device depends on various factors such as film thickness, solvent engineering, fabrication methods, annealing temperature and device architectures which are difficult to compare, still we attempt to compare the obtained Voc of 1-film with the recently reported lead free perovskite light absorbers and found to be superior (Table 1). This high Voc (430mV) of 1-

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film may be attributed either to the 1D-polymeric structure of 1 or the presence of TiO2 blocking layer which reduced the recombination of the transferred electron with the hole present in 1. Previously some lead free perovskites [1,6hexanediammonium bismuth iodide, (CH3NH3)3Bi2I9Clx, (CH3NH3)2CuCl2Br2, (CH3NH3)3Bi2I9)] have been used as light absorbers in perovskite solar cells.

Corresponding Author *Email: [email protected].

ACKNOWLEDGMENTS K. A. would like to thanks to University Grant Commission (UGC) New Delhi, India for providing fellowship (RGNF-D). We sincerely acknowledge Sophisticated Instrumentation Centre (SIC), IIT Indore for providing the characterization facility. S.N.A. would like to acknowledge MHRD, New Delhi. S.M.M. thanks to SERB-DST (Project No. EMR/2016/001113), New Delhi, India for financial support and IIT Indore for research grant. We are thankful to Dr. Shaibal Mukherjee, Discipline of Electrical Engineering, IIT Indore for providing solar simulator and Spectroscopic Ellipsometry analysis facility.

Table 1. Comparison of open circuit voltage of 1 based perovskite solar cells device with contemporary literature on lead-free perovskite based solar cells. Light absorbers

Voc(mV)

References

1,6-hexanediammonium bismuth iodide (HDABiI5)

384

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(CH3NH3)3Bi2I9Clx

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(CH3NH3)2CuCl2Br2

300

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(CH3NH3)3Bi2I9

354

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1D polymer-[(CH3NH3)3Bi2Cl9]n

430

This Work

ASSOCIATED CONTENT Supporting Information available: [Experimental, device fabrication, synthesis, EDX, Spectroscopic ellipsometry, J-V characteristics, Nyquist plots and cyclic voltammetry; Figures S1-S6; Table S1-S4]

REFERENCES

However, bismuth based lead free perovskites shows good stability under atmospheric conditions but the poor efficiency is still remains a challenge this may be due to the rapid crystallization or uncontrolled film morphology of in bismuth based lead free perovskites.29,30,32 Therefore, it is necessary for bismuth based lead free perovskites solar cells to develop the new methods or strategies to control the film morphology to enhance the performance. We have prepared the bismuth based new light absorber which shows good optoelectronic properties and excellent moisture stability. The structure of the (CH3NH3)3Bi2Cl9 perovskite was first time reported by Belkyal et al., in 1997 but to the best of our knowledge for the first time its optical property has been explored by us and employed as light absorber.33,34 Moreover, the nontoxic bismuth had another great advantage over lead based perovskites.

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We have reported the highly stable and lead free 1Dpolymeric chain of 1 as perovskite. 1 shows an excellent stability, moisture resistance and non-toxic behavior which make it superior over lead based perovskites. We have developed a lead free mesoscopic perovskite solar cells (MPSCs) device by employing 1 as light absorber. Although fabricated MPSCs device showed poor efficiency but the obtained circuit voltage of 430mV is remarkable. We believe that the efficiency of circuit voltage of 430mV could be improved by developing fabrication methods, optimizing films thickness, solvent engineering, employing different architectures or new hole/charge extraction materials. Moreover, 1 had a band gap of 2.85eV and polymeric structure which suggest its potential for photodetectors, LED, batteries and supercapacitors.

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CONFLICTS OF INTEREST There are no conflicts to declare.

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Table of contents (TOC)

Fabrication of lead free perovskite solar cells by employing 1D polymer chain of [(CH3NH3)3Bi2Cl9]n (1) as a new light absorber which shows an excellent open circuit voltage of 430 mV with sound air stability.


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ACS Applied Energy Materials

Fabrication of lead free perovskite solar cells by employing 1D polymer chain of [(CH3NH3)3Bi2Cl9]n (1) as a new light absorber which shows an excellent open circuit voltage of 430mV with sound air stability. 254x190mm (96 x 96 DPI)


Design and Synthesis of 1D-Polymeric Chain Based [(CH3NH3

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