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8 protocols using d8 advance

1

Comprehensive Material Characterization

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The surface morphology and chemical composition of the samples were observed and analyzed via the field-emission scanning electron microscope (FE-SEM, Hitachi SU8010, Japan). The XRD (Bruker D8 Advance) patterns of the samples were recorded on a Rigaku Ultima IV with Cu Kα radiation (10° min−1). The thermogravimetry analysis (METTLER, TGA/DSC 1/1100, Switzerland) was recorded under dynamic oxygen flow by heating the samples to 800 °C at a rate of 10 °C min−1. The element content of the samples was analyzed by ICP-OES (Thermo Fisher iCAP6300).
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2

In situ XRD Analysis of Electrochemical Processes

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In situ XRD (operando mode) was carried out using an in situ cell purchased from Rigaku on a D8 ADVANCE powder diffractometer equipped with Co radiation in 0.02° steps over the 2θ range of 17−25° (1.37 s per step, one pattern recorded every ≈12 min). The electrochemical part of the cell is similar to the one described above. The only exception lies in the preparation of the electrode whose slurry was coated on plastic films to be peeled off after drying. The current rate was C/20 (full (dis)charge theoretically achieved in 20 h), allowing us to record an XRD pattern every Δx=0.02. Only selected patterns are shown in Supplementary Fig. 4 for clarity concerns. Electrochemistry was controlled and recorded using a Biologic VMP3.
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3

Characterization of Inorganic Compounds

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All the chemicals required were obtained from Sigma-Aldrich, Alfa Aesar, Spectrochem, and TCI and used without further purification. FT-IR spectra were recorded on a Bruker Alpha II system (ν max in cm−1) on KBr disks. 1H NMR and 13C NMR (400 MHz and 100 MHz respectively) spectra were recorded using a Bruker Avance II-400 spectrometer using CDCl3 as the solvent (chemical shifts in δ with TMS as internal standard). Powder XRD analyses were carried out using a Bruker D8 Advance and Rigaku Ultima IV XRD instrument. Transmission Electron Microscopy (TEM) analysis was carried out using a JEOL JSM 100CX system. Scanning electron microscopy (SEM) and Energy Dispersive X-ray (EDX) analysis were carried out using a JSM-6360 (JEOL) system. X-Ray Photoelectron Spectroscopy (XPS) was performed using a PHI 5000 VersaProbe III system. Thermogravimetric analysis (TGA) was carried out using a Perkin Elmer Precisely STA 6000 simultaneous thermal analyzer. Inductively coupled plasma optical emission spectroscopy (ICP-OES) was carried out using Thermo Scientific™ iCAP™ 7600 instrument. TLC Silica gel 60 F254 (Merck) was used for TLC analysis. Hexane refers to the fraction boiling between 60 and 80 °C.
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4

Comprehensive Materials Characterization Protocol

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Scanning electron microscopy (SEM) graphs were taken by Zeiss SIGMA. Transmission electron microscopy (TEM) coupled with EDS, SAED, and high‐resolution TEM were conducted by FEI Tecnai G2 F30 S‐TWIN. X‐ray diffraction patterns were obtained by Bruker D8 Advance and Rigaku Miniflex600. N2 adsorption–desorption analysis was undertaken by TriStar II 3020. Quantitative elemental analyses were measured by inductively coupled plasma‐atomic emission spectroscopy (Agilent 5110) and Atomic Absorption Spectroscopy (contrAA700). Fourier transform infrared spectroscopy was conducted by Thermo FTIR5700. X‐ray photoelectron spectroscopy (XPS) analyses were carried out by Thermo Fisher Scientific ESCALAB250Xi.
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5

Comprehensive Nanoparticle Characterization

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The NPs synthesized were characterized by different techniques. The structural characterization of the NPs was performed by X-ray powder diffraction analysis using a D8 Advance diffractometer (Rigaku, Tokyo, Japan) equipped with Ge (111) monochromator, CuKα1 radiation, and LynxEye superspeed position detector. The aspects of the NPs obtained were analyzed using scanning/transmission electron microscope, STEM HITACHI HD2700 (HITACHI, Tokyo, Japan), from LIME-INCDTIM, Cluj-Napoca, Romania, cold field emission, operated at 200 kV and coupled with double cut EDX (energy-dispersive X-ray spectroscopy) system, operated at 10−7 pressure. It was used to confirm the elemental distribution in the NPs, and the size distribution was analyzed using Image J (version Java 8). FTIR measurements were performed with a JASCO 6100 FTIR spectrometer (JASCO Deutschland GmbH, Pfungstadt, Germany) in the 4000–400 cm−1 spectral domain with a resolution of 4 cm−1 by using the KBr pellet technique [34 (link)].
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6

Multimodal Characterization of Thin Films

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The surface of the films is controlled in situ with reflection high-energy electron diffractometer fitted with kSA 400 Analytical RHEED system (k-Space Associates, Inc.). This system allows for a 3D representation of the RHEED pattern (Fig. 1) which displays the signal intensity as a third coordinate. Such representation is more informative than the standard 2D representation. X-ray diffraction experiments are carried out with Bruker D8 Advance and Rigaku SmartLab 9kW spectrometers (CuKα X-ray source). Rutherford backscattering spectra are recorded for He ions with the energy 1.7 MeV. Magnetic properties are measured with SQUID magnetometer Quantum Design MPMS XL-7. Transport measurements are carried out using Lake Shore 9709A Hall effect measurement system.
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7

Extensive Characterization of Perovskite Solar Cells

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FE-TEM images were photographed by a JEM-2100F (JEOL Ldt., Tokyo, Japan). XRD patterns were acquired from an X-ray diffractometer (Advance D8, AXS, Rigaku Corporation, Tokyo, Japan). XPS (ESCALAB 250Xi, Thermo Fisher Scientific, Waltham, Massachusetts, USA) was employed to analyze the chemical elements of the samples. SEM (JSM-IT300, JEOL Ldt., Tokyo, Japan) was used to scan the surface and section of the as-prepared samples. The light-absorption spectra were obtained via UV-vis spectrophotometry (UV3600, Shimadzu Corporation, Tokyo, Japan). The photocurrent-voltage (J-V) characteristics were acquired from an electrochemical workstation (Zahner Company, Kronach, Germany) with a solar light simulator (Oriel Sol3A, Newport Corporation, Irvine, CA, USA), under simulated AM 1.5G illumination, at 100 mW/cm2 intensity. Finally, IPCE (Newport Corporation, Irvine, CA, USA) was employed to study the quantum efficiency of the PSCs. The PL spectra were measured with a fluorescence spectrometer (RF-6000, Shimadzu Corporation, Tokyo, Japan). The EIS analyses were conducted on an electrochemical workstation (Zahner Company, Kronach, Germany) for frequencies of 10 mHz to 10 MHz at a bias of 0.8 V under simulated AM 1.5G radiation (irradiance of 100 mW/cm2) with an alternating current (AC) signal amplitude of 10 mV at room temperature.
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8

Characterization of Ag@SiO2 Core-Shell Nanoparticles

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The TEM images of Ag@SiO2 core-shell nanoparticles were measured by a JEM-2010 FEF transmission electron microscope at an acceleration voltage of 200 KV. X-Ray diffractometer (XRD) images were acquired from an X-ray diffractometer (Advance D8, AXS, Rigaku Corporation, Tokyo, Japan). The SEM images of the surface and cross section of the prepared sample were scanned by a field emission scanning electron microscope (JSM-IT300, JEOL Ldt, Tokyo, Japan). The light-absorption spectra were obtained via UV-vis spectrophotometry (UV3600, Shimadzu Corporation, Tokyo, Japan). The photocurrent-voltage (J-V) characteristics were tested by solar simulator (Oriel Sol3A, Newport Corporation, Irvine, CA, USA) under AM 1.5G illumination at 100 mW/cm2 intensity. Incident photon-to-electron conversion efficiency (IPCE) (Newport Corporation, Irvine, California, USA) was used to investigate the quantum efficiency of the PSC devices. The photoluminescence (PL) spectroscopy of PSCs was tested by fluorescence spectrometer (RF-6000, Shimadzu Corporation, Tokyo, Japan). The electrochemical impedance spectroscopy (EIS) of PSCs was obtained by an electrochemical workstation (Zahner Company, Kronach, Germany) for frequencies of 10 mHz to 10 MHz at a bias of 0.8 V under simulated AM 1.5 G radiation (irradiance of 100 mW/cm2) with an alternating current (AC) signal amplitude of 10 mV at room temperature.
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