Supporting Information. Chlorine in PbCl 2 -Derived Hybrid-Perovskite Solar Absorbers
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1 Supporting Information Chlorine in PbCl 2 -Derived Hybrid-Perovskite Solar Absorbers Vanessa L. Pool, Aryeh Gold-Parker, Michael D. McGehee and Michael F. Toney * SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, CA Stanford University Department of Chemistry, 333 Campus Drive, Stanford, CA Stanford University Department of Materials Science and Engineering, 496 Lomita Mall, Stanford, CA These authors contributed equally. Table of Contents Methods... 2 Sample Preparation... 2 Materials... 2 Substrate Preparation... 2 Solution Preparation and Film Deposition... 2 XANES Experimental Setup... 2 Data Analysis... 3 ATHENA Software... 3 XANES Spectra and Linear Combination Fitting... 3 Determination of Cl Concentration... 4 Table S1: Cl:Pb Atomic Ratio for ex-situ annealed samples on SiN windows... 5 MAPbCl 3 as a Standard... 5 Table S2: Triiodide and Trichloride Perovskite Crystal Structures... 5 References
2 Methods Sample Preparation Materials All chemicals, unless otherwise noted, were commercially sourced and used as received without further purification. Dry solvents were Sigma Aldrich Sure/Seal solvents and used as received. PbCl 2 : Aldrich (99.999% purity) MACl: Aldrich M0505, dried under vacuum at 50 C MAI: Dyesol Substrate Preparation Pilkington TEC15 FTO glass was cleaned by sonication in a diluted Extran solution (EMD, EX0996-1), acetone (EMD, AX0115-1), and isopropanol (EMD, PX1835P-4). 0.02M aqueous TiCl 4 was spin-coated on the substrates, which were then dried at 75 C for 15 minutes. The substrates were then sintered to 482 C to convert the layer to TiO 2. FTO/TiO 2 substrates were heated at 120 C before solution deposition to remove surface moisture. 100 nm-thick SiN windows (Norcada NX5200C) were used for transmission experiments. These substrates were UV-ozone cleaned before solution deposition to enhance wetting. Solution Preparation and Film Deposition All spin-coating was performed with solutions and substrates at room temperature. MAPbI 3-x Cl x : 0.88M PbCl 2 and 2.64M MAI were added to DMF in a N 2 glovebox. Solutions were stirred at 75 C for at least 1 hour, until fully dissolved. Films were spin-coated at 2000 rpm for 45s. PbCl 2 : 0.88M PbCl 2 was added to DMSO in a N 2 glovebox. Solutions were stirred at 75 C for at least 1 hour, until fully dissolved. Films were spin-coated at 2000 rpm for 45s. MAPbCl 3 : 0.88M PbCl 2 and 0.88M MACl were added to DMSO in a N 2 glovebox. Solutions were stirred at 75 C for at least 1 hour, until fully dissolved. Films were spin-coated at 2000 rpm for 45s. MACl: MACl powder was evaporated onto substrates in a glass petri dish at 115 C. XANES Experimental Setup All XANES measurements were taken at beamline 4-3 of the Stanford Synchrotron Radiation Lightsource (SSRL), using the Si(111)φ=90 double crystal monochromator. The beam was detuned by 20% to reduce 3 rd harmonic effects. The energy was calibrated by referencing the primary peak of KCl to energy of 2825 ev. 1 Ex-situ annealed samples were deposited on SiN windows and were recorded simultaneously in florescence and transmission geometry. A PIPS solid-state detector was used to measure the florescence signal, and helium-filled ion chambers were used to measure the incident and transmitted intensities. Samples were aligned normal to the x-ray beam to achieve the best transmission signal. This orientation also minimizes the effects of self-absorption in fluorescence data. Given the thickness of the samples and the orientation, the self-absorption effects are negligible. The XANES spectra of the samples deposited on FTO/TiO 2 were measured in florescence only (as the substrates do not transmit x-rays at relevant energies) using a 4-element Vortex detector. 2
3 Data Analysis ATHENA Software All the data analysis was performed in ATHENA, including the averaging, blank silicon nitride window subtraction, normalization, and linear combination fitting (LCF). 2 In the Athena software, normalization is done by fitting the pre-edge region to a linear function and the post-edge to a cubic spline. The edge step height is then calculated as the difference between these functions evaluated at the absorption edge energy. The transmission data were used to calculate the Cl:Pb ratio, and the florescence data were used for the XANES analysis. Multiple scans were averaged to improve the signal to noise ratio. The error was calculated from the scan-to-scan variation. XANES Spectra and Linear Combination Fitting Linear combination fitting (LCF) was used to investigate the state of Cl in the films. Since one speculation was that the Cl remaining in the film was leftover precursor materials, a LCF was performed using PbCl 2 and MACl. This was found to be a very poor match to the Cl signal from the fully annealed sample. Further investigations were done by performing a LCF to the 120min and 0min samples with all three standards: PbCl 2, MACl and MAPbCl 3. In the LCF of the 0min sample, the MACl predominates in the fit leading us to hypothesize that the 0min sample has a significant quantity of MACl (though it could also be a chemical species with a very similar spectrum). LCF to the 120min and the 0min sample as well as the measured spectra are shown in Figure S1. These fits reflect the observation that Cl may be in a Figure S1: Solid lines show the measured Cl K- edge XANES spectra for 120min and 0 min films. Dotted lines show the LCF with combinations of the standards. Figure S2: a. Cl K-edge XANES of samples deposited on FTO/TiO 2 and SiN. b. Cl K-edge XANES of the FTO/TiO 2 and SiN substrates. c. 120min perovskite film versus blank SiN window without normalization. 3
4 MAPbCl 3 -like state in the fully annealed perovskite. It is also noted that LCF does not provide a unique solution; thus, all fits must be seen within that context. We also measured perovskite samples deposited on FTO/TiO 2 in order to verify that the XANES is not substrate dependent. A comparison of the XANES of samples on SiN and FTO/TiO 2 is shown in Figure S2. The spectral shape is seen to be the same within experimental error. Determination of Cl Concentration In order to quantify the amount of Cl present in the perovskite film, the Cl K-edge and Pb M 3 - edge were measured in a continuous scan and the edge steps compared. The data taken in transmission mode were used for this calculation to avoid potential inaccuracies introduced by self-absorption effects. A blank substrate was also measured with the same statistics as the 120 min film. A very small Cl signature was measured on the substrates, considerably smaller and dissimilar in shape to that of the perovskite films as shown in Figure S2. To avoid artificially inflating the Cl quantity, the spectrum from the blank substrate was subtracted from the data. After the spectrum was corrected in this manner, the ratio of the Cl to Pb edge jump was calculated. The edge step height ratio (h Cl/ h Pb ) is proportional to the ratio of the number of Cl atoms to Pb atoms (N Cl /N Pb ). A standard of PbCl 2, assumed to be 2 Cl atoms per Pb atom, was used to calibrate the proportionality factor. The calculated values of Cl/Pb can be found in Table S1. The errors listed were determined by looking at scan-to-scan variation for a given film. These measurements are representative of the sample as a whole as the beam spot size, or sampling size, was 1mm by 1mm, which covered most of the measurable film. A sample prepared on the more standard FTO/TiO 2 substrate was measured in-situ with florescence yield and the un-normalized XANES from this experiment are shown in Figure S3. These data were treated in the same manner as the transmission data to determine a Cl/Pb ratio. However, these fluorescence measurements are not strictly quantitative for two reasons. First, possible self-absorption in samples with large concentrations of Cl (like PbCl 2 ) makes calculating the constant of proportionality difficult. For this reason, the values have been scaled by the 0 min value determined by the transmission data. The second reason is that subtraction of the blank substrate is not straightforward for fluorescence measurements, as it is in transmission. The substrate can contribute to the signal, however the contribution will be less then that of a blank since the signal will have to pass though the sample and will be partially absorbed. By doing a simple subtraction as we have done here we are overcorrecting. For the fluorescence measurements, these approximations introduce additional error. Thus, although the transmission (ex-situ) measurements are quantitative, the fluorescence (in-situ) measurements are not strictly quantitative. Figure S3: Un-normalized in-situ XANES showing the Pb M 4 -edge and the Cl K-edge. Inset: close-up of Cl K-edge XANES region. 4
5 Table S1: Cl:Pb Atomic Ratio for ex-situ annealed samples on SiN windows Anneal Time (min) Cl:Pb Atomic Ratio Error in Cl:Pb Ratio MAPbCl 3 as a Standard The standard MAPbCl 3 was chosen because it is the closest likeness of a small concentration of Cl substitution in I lattice sites. It is, however, an imperfect standard since the MAPbCl 3 and MAPbI 3 structures are rather different (Table S2). 3 This discrepancy in lattice parameters, and the difference in I rather than Cl for the majority of the sites, will introduce differences in the spectra. Modeling is required to know to what extent the spectra would change. For these reasons, MAPbCl 3 is used only to gain clues as to the form of Cl rather than to identify it as a given chemical species. To specifically identify the final state of Cl in the film, modeling of XANES would be required for Cl substitution on the I lattice site, Cl incorporation in interstitial sites, Cl incorporation on grain boundaries, and Cl at the interface with the substrate. Table S2: Triiodide and Trichloride Perovskite Crystal Structures Chemical Formula Crystal System Space Group Lattice (Å) CH 3 NH 3 PbCl 3 Cubic P m3m a=5.675 CH 3 NH 3 PbCl 3 Tetragonal P 4/mmm a=5.656 c=5.630 CH 3 NH 3 PbI 3 Cubic P m3m a= CH 3 NH 3 PbI 3 Tetragonal I 4/mcm a=8.855 c= References (1) Zhu, F.; Takaoka, M.; Shiota, K.; Oshita, K.; Kitajima, Y. Chloride chemical form in various types of fly ash. Environ. Sci. Technol. 2008, 42, (2) Ravel, B.; Newville, M. ATHENA, ARTEMIS, HEPHAESTUS: Data analysis for X-ray absorption spectroscopy using IFEFFIT. J. Synchrotron Radiat. 2005, 12, (3) Poglitsch, a.; Weber, D. Dynamic disorder in methylammoniumtrihalogenoplumbates (II) observed by millimeter-wave spectroscopy. J. Chem. Phys. 1987, 87,
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