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Copyright WILEY-VCH Verlag GmbH & Co. KGaA, 69469 Weinheim, Germany, 2019.Supporting Informationfor Small, DOI: 10.1002/smll.201904746Low-Cost and Highly Efficient Carbon-Based PerovskiteSolar Cells Exhibiting Excellent Long-Term Operational andUV StabilityNeha Arora, M. Ibrahim Dar,* Seckin Akin, RyusukeUchida, Thomas Baumeler, Yuhang Liu, Shaik MohammedZakeeruddin, and Michael Grätzel*
1 Copyright WILEY-VCH Verlag GmbH & Co. KGaA, 69469 Weinheim, Germany, 2019. Supporting Information Low-cost and highly efficient carbon-based perovskite solar cells exhibiting excellent long-term operational and UV stability Neha Arora 1‡, M. Ibrahim Dar,1‡* Seckin Akin,1,2 Ryusuke Uchida,1 Thomas Baumeler1, Yuhang Liu,1 Shaik Mohammed Zakeeruddin,1 and Michael Grätzel1* Experimental Section Materials All materials were used as received unless stated otherwise. Methods Substrate preparation Fluorine-doped tin oxide (FTO) glass substrates (Nippon Sheet Glass (NSG) 10 Ω/sq) were first patterned by chemical etching using Zn powder and 4M HCl solution. The etched substrates were then thoroughly cleaned by ultrasonication in Hellmanex (2% in deionized water) solution for 30 min, followed by sequential rinsing with de-ionized water, ethanol, and acetone. The substrates were treated with UV–O3 for 15 min to remove the last traces of organic residues. A ∼30 nm-thick blocking layer of TiO2 was subsequently deposited on FTO via aerosol spray pyrolysis at 450 °C from a precursor solution of titanium diisopropoxide bis(acetylacetonate) (75% in 2-propanol) diluted in ethanol (1:9, volume ratio) with oxygen as a carrier gas with sintering at 450°C for 30 min. The mesoporous TiO2 layer was deposited by spin coating TiO2 paste of (Dyesol 30 NR-D) diluted in anhydrous ethanol (1:6 weight ratio) at 4000 rpm for 20 s and consequently sintering of the substrates at 450°C for 30 min under dry air flow. The as-prepared mesoporous substrates were transferred into a dry air glove box after cooling down to 150 °C for perovskite deposition. Device fabrication
2 Perovskite film deposition: The perovskite deposition was carried out in a dry air glove box under controlled atmospheric conditions with humidity <2% (dew point was about −30 °C). Perovskite films were deposited using a single-step deposition method from the precursor solution containing FAI (1.0 M) (Greatcell Solar), PbI2 (1.1 M) (TCI), MABr (0.2 M) (Greatcell Solar) and PbBr2 (0.2 M) (TCI) in anhydrous dimethylformamide (99.8%, Acros) / dimethylsulphoxide (99.7%, Acros) (4:1 (v:v)). Thereafter, CsI (abcr, GmbH, ultra-dry; 99.998%), (5% volume, 1.5 M DMSO) was added to the precursor solution. The spin-coating procedure was performed on the mp-TiO2 films in a two-step program at 1000 and 6000 rpm for 10 and 30 s, respectively. During the second step, 100 μL of chlorobenzene was dropped onto the spinning substrate 10 s prior to the end of the spinning. This was followed by annealing the films at 100 °C for 45 min in the dry-air glove box. Hole conductor deposition: After cooling down to room temperature, the hole transport material layers were coated via solution process by the following methods. CuSCN solution was prepared by dissolving 35 mg CuSCN salt (99%, Sigma-Aldrich) in 1 mL of diethyl sulfide (98%, TCI) after constant stirring at room temperature for 30 min. To deposit a thin and uniform film of CuSCN, 35 μL of a CuSCN solution was drop cast within 1-2 seconds on the substrate containing perovskite film spinning at 5000 rpm, and the substrate was allowed to spin for 30 seconds. 2,2’,7,7’tetrakis(N,N dipmethoxyphenylamine) 9,9spirobifluorene (spiro-MeOTAD, Merck) solution (70 mM in chlorobenzene) was spin coated at 4000 rpm for 20 s. Spiro-MeOTAD was doped with bis(trifluoromethylsulfonyl)imide lithium salt (Li-TFSI, Sigma-Aldrich), tris(2-(1H-pyrazol-1-yl)-4-tert-butylpyridine)-cobalt(III) tris(bis(trifluoromethylsulfonyl)imide) (FK209, Dynamo) and 4-tert-Butylpyridine (TBP, Sigma-Aldrich). The molar ratio of additives for spiro-MeOTAD was 0.5, 0.03, and 3.3 for Li-TFSI, FK209, and TBP, respectively.
3 Deposition of back contacts: Finally, the room-temperature processed carbon paste (Greatcell Solar) was coated on the CuSCN-coated perovskite film using the doctor-blading method. The carbon coating procedure was carried out in an ambient atmosphere. For gold deposition, 80 nm of the gold counter electrode was deposited by thermal evaporation under high vacuum. Deposition of a thin layer of SnO2 layer by low-temperature ALD (atomic layer deposition) onto mesoporous TiO2 The atomic layer-by-layer deposition of SnO2 was carried out at 118 °C using successive pulses of tetrakis(dimethylamino)- tin(IV) (TDMASn) (99.99%-Sn, Strem Chemicals INC) and ozone using nitrogen as a carrier gas in a Savannah ALD 100 instrument (Cambridge Nanotech Inc.). The Sn (TDMASn) precursor was held at 65 °C. Oxygen gas (99.9995% pure, Carbagas) was used for the production of ozone by an ozone generator (AC-2025, IN USA Incorporated). Nitrogen (99.9999% pure, Carbagas) was employed as a carrier gas. Photovoltaic device characterization The current-voltage (J-V) characteristics of the perovskite devices were recorded with a digital source meter (Keithley model 2400). A 450 W xenon lamp (Oriel) was used as the light source. The spectral mismatch between AM1.5G and the simulated illumination was reduced by the use of a Schott K113 Tempax sunlight filter (Praezisions Glas and Optik GmbH). Before each measurement, the exact light intensity was determined using a calibrated Si reference diode equipped with an infrared cutoff filter (KG-3, Schott). The voltage scan rate was 50 mV s-1. The photo-active area of 0.16 cm2 was defined using a dark-colored metal mask. External quantum efficiency (EQE) measurements were made using a LED light source (Ariadne EQE from Cicci Research). Time-resolved photoluminescence Time-resolved photoluminescence spectra were recorded on a spectrofluorometer Fluorolog 322 working in a single-photon counting mode by exciting the samples with picosecond pulsed diode laser head NanoLED-405LH (Horiba) which emits <200 ps duration pulses at
4 406 nm with a repetition rate of 1 MHz and pulse energy about 11 pJ was used as an excitation source. SEM analysis Field emission scanning electron microscopy (Merlin) was employed to examine the morphology and thickness of carbon and perovskite films. An electron beam accelerated to 3 kV was used with an in-lens detector. Raman studies Raman spectral measurements were carried out on a LabRAM HR (UV) system using an argon-ion laser with an excitation wavelength of 514 nm. Sheet resistance The sheet resistance of the unannealed carbon layer deposited on a non-conducting glass substrate was measured using a four-point probe technique. Long-term Operational and UV-stability Photo-stability tests were carried out at a maximum power point under one-sun illumination at 60 °C using a home-built electronic board with an eight-channel maximum power point capability. Equivalent sun intensities were calibrated using a calibrated Si reference diode equipped with a KG-3 filter. The setup was calibrated periodically using a Keithley 2602B source-measuring unit. UV-stability measurements were carried out using a home-built setup containing. The UV-light source consisted of an array of five Philips TL-D 18W tubes (wavelength = ~340-390 nm) was powered by a constant current. The un-encapsulated devices were exposed to UV radiation of 10 W/m2 continuously, and the photovoltaic efficiencies were periodically recorded under AM1.5 simulated sunlight.
5 Figure S1. Cross-section SEM micrograph displaying film composed of carbon sheets.
6 Figure S2. Top-view SEM micrograph of 17B perovskite film. Figure S3 Cross-section SEM micrograph of the Spiro-MeOTAD based PSC involving 17B perovskite film.
7 Figure S4. Current-voltage characteristics of spiro-OMeTAD based 17B-PSC measured under standard simulated AM1.5 illumination at a scan rate of 50 mV/s (reverse scan, with an illumination area of 0.16 cm2).
8 Figure S5. Current-voltage characteristic for CuSCN/C PSC measured under standard simulated AM1.5 illumination at a scan rate of 50 mV/s (reverse scan, with an illumination area of 0.16 cm2).
9 Figure S6. External quantum efficiency for CuSCN/C PSC with the integrated current density value.
10 Figure S7. J-V characteristics of the best performing 10B/CuSCN-based device with ~200 µm thick carbon layer as a back contact recorded at a scan rate of 50 mV/s (reverse scan, with an illumination area of 0.16 cm2).
11 Figure S8. Photovoltaic metrics for 10 (10B/CuSCN) devices based on ~200 µm thick carbon layer as the back contact, average JSC value of 21.9±0.55 mAcm-2, VOC 986±2.3 mV, FF 76.5±1.25%, and PCE 16.7±0.40%. 202224 Jsc (mAcm-2)9809901000 Voc (mV)727680 FF (%)16.017.6 PCE (%)
12 Figure S9. EQE as a function of monochromatic wavelength and the integrated current density obtained from the respective EQE spectrum of 10B/CuSCN/C PSC. (Integrating the overlap of the EQE spectrum with the AM 1.5G solar photon flux yielded a photocurrent density of 21.7 mA/cm2 which is in excellent agreement with the photocurrent density value obtained from the J-V measurement (21.9 mA/cm2). 400500600700800020406080100 CuSCN/C (Carbon thickness ~200 µm)Wavelength (nm)EQE (%)0510152025Integrated current (mA cm-2)
13 Figure S10. J-V characteristics of 10B-based PSCs measured under standard simulated AM1.5 illumination at a scan rate of 50 mV/s (reverse scan, with an illumination area of 0.16 cm2) corresponding to the devices based on the FTO/c-TiO2/m-TiO2/Perovskite/Spiro/Au architecture. Inset: PV metrics derived from the J-V curve.
14 Figure S11. J-V characteristics of 10B-based PSCs measured under standard simulated AM1.5 illumination at a scan rate of 50 mV/s (reverse scan, with an illumination area of 0.16 cm2) corresponding to the devices based on FTO/c-TiO2/m-TiO2/SnO2(ALD)/Perovskite/Spiro/Au architecture. Inset: PV metrics derived from the J-V curve. Figure S12: UV-stability of PSCs based on ITO/SnO2/Perovskite/Spiro/Au architecture. The data presented is a summary of 3 devices with error bar. 010203040506070800.00.20.40.60.81.0PCE (a.u.)Time (h)
15 Figure S13. Maximum power point tracking for 60 s, yielding stabilized efficiencies of 18.02% for FTO/c-TiO2/m-TiO2/Perovskite/CuSCN/C based device. 01020304050141516171819PCE (%)Time (s) 18.02%
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