In situ (S)TEM experiments were carried out using an aberration-corrected JEOL ARM 300F at 300 kV in STEM and TEM modes. The real-time diffraction pattern, dark-field TEM images, and atomic HAADF-STEM images were recorded using a JEOL ARM 300F with a double-tilt holder provided by the ZEPTools Technology Company. The acquisition parameters of the real-time diffraction pattern were 4,096 × 4,096 pixels for each frame and 7 frames/s. The dark-field TEM images related to the applied electric field were completed in TEM mode with the microscope equipped with a OneView camera (Gatan). The images were recorded with 4,096 × 4,096 pixels for each frame and 25 frames/s; the corresponding temporal resolution was 0.04 s. Quantitative measurements of the mechanical loads were performed using an FEI F20 microscope operated at 200 kV in TEM mode and equipped with a OneView camera together with a Hysitron system (PI 95). The images were recorded with 1,024 × 1,024 pixels for each frame and 10 frames/s from the OneView camera; the corresponding time resolution was 0.1 s. The atomic HAADF-STEM images were recorded with 2048×2048 pixels for each frame, and the dwell time of each pixel was 4 μs.
Arm300f
Manufactured by JEOL
Sourced in Japan
The ARM300F is a high-resolution analytical electron microscope (AEM) designed and manufactured by JEOL. It features a field emission electron gun and advanced imaging and analytical capabilities. The ARM300F is intended for materials science research, nanotechnology, and other applications requiring high-resolution microscopy and analysis.
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Lab products found in correlation
S 4800, by Hitachi (3 mentions)
F20 microscope, by Thermo Fisher Scientific (2 mentions)
D max 2500n, by Rigaku (2 mentions)
Icpe 9000, by Shimadzu (2 mentions)
Jem 2100f, by JEOL (2 mentions)
Gatan oneview camera, by Ametek (1 mentions)
Sdt q600, by TA Instruments (1 mentions)
K2 summit, by Ametek (1 mentions)
Escalab220i xl electron spectrometer, by VG Scientific (1 mentions)
Asap 2460, by Micromeritics (1 mentions)
Escalab220i xl, by VG Scientific (1 mentions)
D max 2550 5, by Rigaku (1 mentions)
Tristar 3000 system, by Micromeritics (1 mentions)
Jem 2100f transmission electron microscope, by JEOL (1 mentions)
Magellan 400 microscope, by Thermo Fisher Scientific (1 mentions)
Uv 3600 shimadzuuv vis nir spectrometer, by Shimadzu (1 mentions)
Agilent 725, by Agilent Technologies (1 mentions)
Fv1000 microscope, by Olympus (1 mentions)
13 protocols using arm300f
1
In situ (S)TEM characterization techniques
2
In-situ TEM Experiments with Quantitative Mechanical Measurements
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In situ TEM experiments were carried out on a JEOL ARM 300 F instrument at 300 kV in either TEM or STEM mode. Experiments were also partly performed in an FEI F20 microscope operated at 200 kV in TEM mode together with a Hysitron system (PI 95) for quantitative measurement of the mechanical loads. However, for Hysitron holder, the stability is too poor to allow us get any atomic resolution because the mechanical force measurement requires feedback that causes relatively larger vibrations. For better stability and resolution, the real-time diffraction patterns, high-resolution TEM images, and atomically resolved STEM images were recorded on a JEOL ARM 300 F with a PicoFemto double-tilt TEM-STM holder provided by ZepTools Technology Company. A tungsten tip acted as an indenter, and was precisely controlled by a piezoelectric system. A STEM image was obtained each time the tungsten tip moved forward for time-lapse STEM images with a convergence angle of 18 mrad and collection angles of 54–220 mrad.
3
In Situ Heating TEM Characterization
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Two TEMs were used for in situ heating studies: Thermofisher Titan S/TEM (Thermo Fisher Scientific Ltd., Hillsboro, OR, USA) equipped with a Bruker Xflash 6 T | 30 energy-dispersive X-ray (EDX) spectrometer (Bruker, Billerica, MA, USA) and an aberration-corrected JEOL ARM300F (JEOL Ltd., Tokyo, Japan). Both TEMs were operated with an accelerating voltage of 300 kV. The Wildfire heating holders (DENSsolutions, Delft, Netherlands) were used for heating the NPs during in situ observations. Typical electron fluxes used for in situ imaging were in the range of 200−6000 e− Å−2 s−1. Image series were acquired with two different cameras: a Gatan K2 IS camera (Gatan Inc., Pleasanton, CA, USA) on the Thermofisher Titan S/TEM and a Gatan OneView camera (Gatan Inc., Pleasanton, CA, USA) on the JEOL ARM300F. Inverse FFT images in Fig. 1c were obtained by separately filtering and then combining fcc and B2 spots in FFT patterns in Fig. 1a , and the same processing was used for Supplementary Figs. 3 , 4 , 10 , and 14 .
4
Multiscale Characterization of Fiber Samples
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Optical images were collected by a Leica optical microscope. XRD spectra were acquired with a Rigaku Smartlab workstation using CuKα (1.54 Å) radiation. Thermogravimetric analysis was performed on a SDT Q600 instrument (TA Instruments, Inc.). Experiments were carried out on ~2 mg fiber samples and the heating rate of 10 °C min−1 under a 70 mL min−1 air flow. TEM and cross-sectional TEM images were collected using a JEOL ARM300F transmission electron microscope. Samples for top-view TEM images were obtained by placing the fibers on water and transferring them onto TEM grids.
5
Atomic Structure Imaging of LAO/STO/Al2O3 Sample
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The atomic structure imaging was conducted on LAO/STO/Al2O3 sample by using Cs-corrected TEM (JEOL-ARM300F) operated at 300 kV. Convergence angle for both STEM and EDS acquisition was 35.63 mrad. Collection angle for HAADF imaging was 68 to 280 mrad. Energy-dispersive x-ray spectrometer with a detectable area of 100 mm2 was used in STEM imaging mode. EDS maps with a total number of 3020 frames were acquired with a speed of 0.655 s per frame with 256 by 256 pixels. The specimen drift was corrected during acquisition. Each elemental map is constructed by integrating the signal from La-Lα, Sr-Lα, Al-Kα, and Ti-Kα characteristic x-rays, respectively. The EDS maps in Fig. 2 were processed by the Wiener filter to minimize random noise, and the averaged EDS profiles in fig. S1 were obtained from the maps without filtering, which do not contain artifact from filtering.
6
Multislice TEM Image Simulation
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TEM image simulations were produced using the QSTEM multislice code,38 using 20 slices and a simulation pixel size of 0.0052 nm (re-binned 5× to the experimental pixel size of 0.026 nm). The following imaging parameters were used, in order to match the AC-TEM experiments acquired at a low doses per image (JEOL ARM300F): 80 kV accelerating voltage; −0.107 nm defocus (Scherzer); 5 nm defocal spread; 0.517 μm Cs; 1.7 mm Cc; 41.65 mrad α; 3.371 nm, 82.75° C12; 0.0982 μm, 33.55° C21; 0.0595 μm, −16.59° C23. Poisson noise due to a finite electron dose was applied with the intensity of each pixel calculated as I(x,y) = Poisson random[Isim(x,y)DΔxΔy], where Isim(x,y) is the image intensity resulting from the multislice simulation, D is the electron dose per image (4.6 × 104 e− nm−2) and ΔxΔy is the pixel size.
7
Atomic-Scale Elemental Mapping via STEM-EELS
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STEM-EELS investigations were performed in a probe-corrected FEI Titan³ G2 60–300, operated at 300 kV. The microscope is equipped with a Gatan Imaging Filter (GIF) Quantum with a Gatan K2 Summit direct-electro-detection camera. Spectrum images are acquired with a convergence angle of 19. 6 mrad and a collection angle of 25 mrad, with a dispersion of 0.1 eV/ch with a pixel size of 0.4 A and a dwell time of 10 ms per pixel for 300 × 200 pixels. Spectra in Fig. 1A are summed over 45 * 25 pixels.
For Fig.S10, a 300 kV field emission TEM (JEOL ARM300F) equipped with a double CS-corrector was used in this study to acquire the high-spatial elemental maps. Two windowless Energy-dispersive X-ray spectroscopy (EDXS) detectors, each of which has an active area of 100 mm2, are equipped on the microscope, which is very close to the specimen with a high solid angle (1.7 sr).
For Fig.S10, a 300 kV field emission TEM (JEOL ARM300F) equipped with a double CS-corrector was used in this study to acquire the high-spatial elemental maps. Two windowless Energy-dispersive X-ray spectroscopy (EDXS) detectors, each of which has an active area of 100 mm2, are equipped on the microscope, which is very close to the specimen with a high solid angle (1.7 sr).
8
Comprehensive Characterization of Catalytic Materials
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The powder X-ray diffraction (XRD) patterns were recorded on a Rigaku D/max-2500n diffractometer with Cu Kα radiation (λ = 1.5418 Å) at 40 kV and 200 mA. The morphologies and microstructures of the samples were measured on the transmission electron microscopy (TEM) (JEM-2100F, JEOL, Japan) and the scanning electron microscopy (SEM) (HITACHI S-4800, Japan). Element mapping was characterized on TEM equipped with Oxford detection. X-ray photoelectron spectroscopy (XPS) measurements were performed on a VG Scientific ESCALab220i-XL electron spectrometer using 300 W Al kα radiation. Inductively coupled plasma atomic emission spectroscopy (ICP-AES) was conducted on a Shimadzu ICPE-9000 to confirm the loading content of metal on the catalysts. The AC HAADF-STEM images were carried out in a JEOL ARM300F at 300 kV, equipped with a probe spherical aberration corrector. Brunauer–Emmett–Teller (BET) surface areas were measured by N2 adsorption-desorption isotherms at 77 K with a Micromeritics ASAP 2460 instrument. The HAADF imaging and EELS mapping were both performed using a Nikon HERMES-100 aberration-corrected scanning transmission electron microscope under 60 kV accelerating voltage with a ~22 pA probe. The probe convergence semi-angle, HAADF collection semi-angle, and EELS collection semi-angle is 32 mrad, 75–210 mrad, and 0–75 mrad, respectively.
9
Comprehensive Characterization of Advanced Materials
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The morphologies and structures of the samples were performed on transmission electron microscopy (TEM) (JEM-2100F, JEOL, Japan) and scanning electron microscopy (SEM) (HITACHI S-4800, Japan). Element mapping was recorded on TEM equipped with Oxford detection. The powder X-ray diffraction (XRD) patterns were characterized on a Rigaku D/max-2500n diffractometer with Cu Kα radiation (λ = 1.5418 Å) at 40 kV and 200 mA. X-ray photoelectron spectroscopy (XPS) measurements were measured on a VG Scientific ESCALab220i-XL electron spectrometer using 300 W Al kα radiation. Inductively coupled plasma atomic emission spectroscopy (ICP-AES) was employed with Shimadzu ICPE-9000 to confirm the loading content of metal on the catalysts. The AC HAADF-STEM images were performed on JEOL ARM300F at 300 kV, equipped with a probe spherical aberration corrector. 1H and 13C NMR spectra were acquired via a Bruker Advance III HD-400 MHz spectrometer with a BFO smart probe.
10
Electron Microscopy Imaging Protocol
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Microscopy for imaging and condition development was performed on two microscopes. A JEOL ARM-200F cold FEG, Cs probe corrected STEM at 80 or 200 kV acceleration voltage, 20-21 mrad convergence angle, using an annular dark field detector at 8 cm camera length, resulting in inner and outer collection angles of 33 and 120.77 mrad, respectively for LAADF imaging and 72.80 and 235.75 mrad for HAADF imaging. A JEOL ARM-300F Cs probe corrected STEM at 300 kV was used for imaging condition development. Both room temperature and cryogenic conditions were examined, and the cryogenic conditions did not noticeably reduce the beam sensitivity of the FAPbI3 thin films, so all imaging was done at room temperature. Similarly, no noticeable difference in beam sensitivity was found between 200 and 300 kV acceleration voltage, but the material was found to damage faster at 80 kV.
All imaging presented in the manuscript was at 200 kV. All alignments and focusing were done away from the areas imaged to reduce electron beam-induced damage to the material. All micrographs were obtained without tilting the sample to reduce the beam damage.
The specific image acquisition conditions for all images are listed in Table S1.
All imaging presented in the manuscript was at 200 kV. All alignments and focusing were done away from the areas imaged to reduce electron beam-induced damage to the material. All micrographs were obtained without tilting the sample to reduce the beam damage.
The specific image acquisition conditions for all images are listed in Table S1.
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