XRD measurements were performed with a Bruker-AXS D8 Discover Diffractometer. Bruker-AXS D8 Discover Diffractometer is configured in parallel beam geometry with Cu Ka radiation. It should be noted we used the scraped powder from the substrates for XRD measurement to exclude the impact of strain effect on the lattice constant40 (link). We have shown that thermal annealing could induce strain in perovskite films grown on ITO substrates, while scraped powders are strain free40 (link). The small amount of power gave wide XRD peaks. As shown in Supplementary Fig. 5 , the full width at half maximums for the XRD peaks of perovskite thin films deposited by both spin coating and blade-coating process are comparable to those of perovskite single crystals in literature24 (link). No notable XRD peak shift was observed within its resolution limit after adding 5% excess metal ions into perovskite thin films. In addition, the blade-coated perovskite film with 5% Sr2+ showed obvious orientation change relative to the pure MAPbI3 film.
Axs d8 discover diffractometer
Manufactured by Bruker
Sourced in Germany, United States
The AXS D8 Discover diffractometer is a versatile X-ray diffraction (XRD) instrument designed for materials analysis. It provides accurate phase identification and quantification, as well as detailed structural characterization of a wide range of materials. The diffractometer features advanced optics and detectors to deliver high-quality data for research and industrial applications.
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Lab products found in correlation
Nanostar system, by Bruker (1 mentions)
Feg 250, by Thermo Fisher Scientific (1 mentions)
Dimension edge, by Bruker (1 mentions)
Rtespa 300, by Bruker (1 mentions)
Libra 120, by Zeiss (1 mentions)
Tecnai f20 tem microscope, by Thermo Fisher Scientific (1 mentions)
Scios 2, by Thermo Fisher Scientific (1 mentions)
Digital optical microscope, by Keyence (1 mentions)
Bx61 microscope, by Olympus (1 mentions)
Jem 2010 microscope, by JEOL (1 mentions)
Arm 200, by JEOL (1 mentions)
10 protocols using axs d8 discover diffractometer
1
XRD Characterization of Perovskite Films
2
Characterizing Diamond and MoS2 Films
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Scanning electron microscopy (SEM) was performed using FEI FEG250 with resolution of 1.2 nm equipped with SE and BSE detector. The surface morphology of the diamond and MoS2 films was probed by atomic force microscopy (AFM) in a tapping mode (Bruker, Dimension Edge), using an etched silicon probe (Bruker, RTESPA - 300).
The crystallographic structure and orientation of the films were examined by X-ray diffraction (XRD) (CuKα) in the classical Bragg–Brentano and in the grazing-incidence configuration using BRUKER AXS D8 DISCOVER diffractometer with a rotating Cu anode.
The grazing-incidence wide-angle X-ray scattering (GIWAXS) measurements were performed using Nanostar system (Bruker AXS, Germany) equipped with IμS microfocus Cu X-ray source (λ = 0.154 nm). The parallel X-ray beam after Montel optics was further collimated using evacuated pinhole collimator equipped with two 550 µm pinholes separated by 1 m. The grazing-angle of incidence of X-ray beam on the sample was set to 0.8°. Reciprocal space maps were measured using an image plate detector at a sample-to-detector distance of 80 mm. All GIWAXS measurements were performed in fully evacuated chamber.
The crystallographic structure and orientation of the films were examined by X-ray diffraction (XRD) (CuKα) in the classical Bragg–Brentano and in the grazing-incidence configuration using BRUKER AXS D8 DISCOVER diffractometer with a rotating Cu anode.
The grazing-incidence wide-angle X-ray scattering (GIWAXS) measurements were performed using Nanostar system (Bruker AXS, Germany) equipped with IμS microfocus Cu X-ray source (λ = 0.154 nm). The parallel X-ray beam after Montel optics was further collimated using evacuated pinhole collimator equipped with two 550 µm pinholes separated by 1 m. The grazing-angle of incidence of X-ray beam on the sample was set to 0.8°. Reciprocal space maps were measured using an image plate detector at a sample-to-detector distance of 80 mm. All GIWAXS measurements were performed in fully evacuated chamber.
3
Nanocrystal Characterization by Electron Microscopy and XRD
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Low resolution transmission electron microscopy (TEM) (Carl Zeiss, Jena, Germany) was conducted on a ZEISS LIBRA 120, operating at 120 kV. Carbon-coated TEM grids from Ted-Pella were used as substrates. High resolution TEM (HRTEM) and scanning TEM (STEM) images were recorded using an FEI Tecnai F20 TEM microscope (FEI company, USA), equipped with a high angle annular dark field (HAADF) detector (FEI company, USA) and operated at 200 kV. Energy-dispersive X-ray spectroscopy (EDS) spectra were obtained in the HAADF-STEM mode. The EDS spectrum of nanocrystals obtained with CuBr2 was gathered using an Auriga Zeiss field-emission scanning electron microscope (SEM) (Carl Zeiss, Jena, Germany) at 5.0–20 kV on a Si wafer. Powder X-ray diffraction (XRD) patterns were obtained with Ni-filtered (2 μm thickness) Cu Kα1 (λ = 1.5406 A) radiation in a reflection geometry on a Bruker-AXS D8 Discover diffractometer (Bruker, Karlsruhe, Germany) operating at 40 kV and 40 mA.
4
Microstructural and Compositional Analysis
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The microstructure and morphology of the samples were conducted using a Hitachi S-4800 field-emission-gun scanning electron microscope (SEM) at 5 kV and 15 kV and a JEM-200CX transmission electron microscope (TEM). The chemical composition was performed by the energy dispersive X-ray spectroscopy (EDS). The high-resolution transmission electron microscopy (HRTEM) observations were investigated on Tecnai F20 TEM under 200 kV acceleration voltage. X-ray diffraction (XRD) analysis was characterized with a Bruker AXS D8 Discover diffractometer (Germany) using Cu-Kα radiation (λ = 1.5406 Å) and the 2θ used in the measurements was range from 5 to 90°. Fourier transform infrared spectroscopy (FT-IR) was measured with a Magna-IR 750 spectrophotometer. X-ray photoelectron spectroscopy (XPS) of the samples were characterized with a PHI 5300 Photoelectron Spectrometer (Perkin Elmer Instruments Co. Ltd., USA). Thermogravimetric analysis (TG-DTA 6200 LAB SYS) was carried out in air from 50 to 800 °C at a heating rate of 10 °C min−1.
5
Microstructural Analysis of Oxidized Powders
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The oxidized powders, sintered substrates, and tribological wear tracks on the sintered substrates were analyzed for their microstructural morphology.
Optical microscopy has been carried out by Keyence digital-optical microscope, (Keyence VHX-950F model, Osaka, Japan). Scanning Electron Microscopy has been carried out by using Thermo Scientific Scios 2 equipment (Waltham, MA, USA) under SEM-BSD and SEM-SE modes using 4kV accelerating voltage. Phase analysis and elemental identification was performed by XRD—Cu Kα radiation using a Bruker AXS D8 Discover diffractometer (Billerica, MA, USA) equipped with Göbel-mirror and a scintillation detector.
Optical microscopy has been carried out by Keyence digital-optical microscope, (Keyence VHX-950F model, Osaka, Japan). Scanning Electron Microscopy has been carried out by using Thermo Scientific Scios 2 equipment (Waltham, MA, USA) under SEM-BSD and SEM-SE modes using 4kV accelerating voltage. Phase analysis and elemental identification was performed by XRD—Cu Kα radiation using a Bruker AXS D8 Discover diffractometer (Billerica, MA, USA) equipped with Göbel-mirror and a scintillation detector.
6
MAPbI3 Single Crystals Growth
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The MAPbI3 thin single crystals were grown by a space confined lateral crystal growth method reported previously27 (link). MAPbI3 solution in GBL with a concentration of 1.6 M was inserted into two substrates and then placed on a 60 °C hot plate. The temperature was gradually increased to 120 °C for crystal growth. The polarized optical microscopy of the single crystals was performed on an Olympus BX61 microscope in reflection mode with a crossed Nicols configuration. The XRD pattern was measured with a Bruker-AXS D8 Discover Diffractometer.
7
Characterizing Silver Nanoparticle Structure
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The crystal structure and purity of the synthesized silver nanoparticles were determined using X-ray diffraction (XRD) analysis performed with (XRD, D8, Bruker, Germany. Tests were held using a Bruker AXS D8 DISCO-VER diffractometer operating at a voltage of 35 kV.
8
Quantifying Crystal Orientation with XRD
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The diffractograms were recorded on a Bruker-AXS D8 Discover diffractometer. The X-ray beam was produced in a sealed copper tube at 40 kV and 40 mA. The 500-μm beam with a CuKα1
wavelength (1.5405 Å) was collimated and parallelized using two crossed-coupled Göbel mirrors.
The X-ray diffraction data were collected using a Vantec 500 two-dimensional detector in the 3-40° 2.θ range. The samples were placed perpendicular or parallel to the X-ray beam.
The azimuthal intensity profiles were used in the calculation of the Herman's orientation factor defined by (Hermans, Hermans, Vermaas, & Weidinger, 1946) :
Where 𝑓 is the crystal chain axis orientation factor and 𝜒 is the angle between the chain axis and the reference direction. The value of 𝑐𝑜𝑠 E 𝜒 is computed from the azimuthal angular distribution of XRD intensity profile by:
Where 𝐼(𝜒) Is the angular intensity profil from the XRD pattern. The degree of orientation 𝑓 is the first term in the expansion of an orientation distribution function which depends on the angle between the chain axis and the reference direction. 𝑓 is equal to 0 for random orientation and to 1 for a perfect alignement (Kim, Oh, & Islam, 2012) .
wavelength (1.5405 Å) was collimated and parallelized using two crossed-coupled Göbel mirrors.
The X-ray diffraction data were collected using a Vantec 500 two-dimensional detector in the 3-40° 2.θ range. The samples were placed perpendicular or parallel to the X-ray beam.
The azimuthal intensity profiles were used in the calculation of the Herman's orientation factor defined by (Hermans, Hermans, Vermaas, & Weidinger, 1946) :
Where 𝑓 is the crystal chain axis orientation factor and 𝜒 is the angle between the chain axis and the reference direction. The value of 𝑐𝑜𝑠 E 𝜒 is computed from the azimuthal angular distribution of XRD intensity profile by:
Where 𝐼(𝜒) Is the angular intensity profil from the XRD pattern. The degree of orientation 𝑓 is the first term in the expansion of an orientation distribution function which depends on the angle between the chain axis and the reference direction. 𝑓 is equal to 0 for random orientation and to 1 for a perfect alignement (Kim, Oh, & Islam, 2012) .
9
X-ray Characterization of Materials
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X-ray reflectivity (XRR) and X-ray diffraction (XRD) measurements were done using a D8-Discover Bruker AXS diffractometer equipped with a Cu-Kα source/Goebel mirror (Bruker Corporation, Billerica, MA, USA) and eventually soller slits at the primary beam, and with variable slits and detector at the secondary path.
10
Comprehensive Materials Characterization by XRD, TEM, SEM, and STEM
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X-ray diffraction (XRD) analyses were performed by using a D8-Discover Bruker AXS diffractometer, equipped with a Cu Kα source, in symmetric configuration (source and detector move by the same incremental angle). Transmission Electron Microscopy (TEM) and Selected Area Electron Diffraction analyses (SAED) were done using a JEOL JEM 2010 microscope operating at 200 kV. Field Emission Scanning Electron microscopy (FE-SEM) images were obtained by using a ZEISS VP 55 microscope equipped with Energy Dispersive X-ray analyses (EDX) INCA-Oxford windowless detector. STEM analysis are obtained using a Jeol ARM200 equipped with a cold FEG electron source, CEOS condenser aberration corrector and 100 mm2 Jeol EDXS detector. Some images are acquired in STEM mode in Z-contrast configuration. EDXS profiles are extracted by a 730 × 180 nm spectrum image across the whole thickness, with 7 nm pixel size, and 0.1 s pixel time. The scanned area was selected in a thicker region of the sample in order to increase and average the signal.
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