Themis z microscope

Scanning electron microscopy (SEM) images were acquired on a Zeiss LEO 1530 field-emission microscope with a gun voltage of 5 kV and a working distance of ~3.5 mm. X-ray photoelectron spectroscopy was acquired by Thermo Scientific K-alpha XPS instrument. Atomic force microscopy (AFM) topography was obtained using an XE-70 Park System. Device corrosion area percentage were statistically analyzed by ImageJ. Four-dimensional scanning transmission electron microscopy (4D-STEM) was performed using Thermo Fisher Scientific Themis Z STEM operated at 300 kV and equipped with an electron microscopy pixel array detector (EMPAD) to acquire nano-diffraction patterns from different sampling areas within the films^{48 (link)}. The intensity variance of acquired nano-diffractions was calculated^{49 (link)}. EDS was performed using FEI Themis Z microscope at 300 kV equipped with four Super-X detectors, and the chemical composition of amorphous films was obtained by analyzing EDS spectra using FEI Vlox software and Kα energies for Ti, Cl, and O. The presence of crystalline phases within the amorphous matrix was investigated by observation of film using low angle annular dark field (LAADF) STEM imaging, including diffraction contrast.

All UV-vis absorption spectra of the nanoclusters dissolved in CH₂Cl₂ were recorded using an Agilent 8453 diode array spectrometer.
The dynamic light scattering (DLS) of each metal complex sample was recorded using a Malvern Zetasizer Nano ZS instrument.
Electrospray ionization mass spectrometry (ESI-MS) measurements were performed by using a Waters XEVO G2-XS QTof mass spectrometer. The sample was directly infused into the chamber at 5 μL min⁻¹. For preparing the ESI samples, nanoclusters were dissolved in CH₂Cl₂ (1 mg mL⁻¹) and diluted (v/v = 1 : 1) with CH₃OH.
Thermogravimetric analysis (TGA) was carried out on a thermogravimetric analyzer (DTG-60H, Shimadzu Instruments, Inc.) with 10 mg of the sample in a SiO₂ pan at a heating rate of 10 K min⁻¹ from room temperature to 1073 K.
The high angle annular dark field scanning transmission electron microscopy (HAADF-STEM) technique was performed by using a FEI Themis Z microscope. The electron beam energy was 200 kV. The HAADF-STEM image was obtained using Thermo Scientific Velox software using 1024 × 1024 pixels and the dwell time was set to 10 μs.

Transmission electron microscopy images were collected using a Hitachi HT7700 microscope operated at 100 kV. High-angle annular dark field scanning transmission electron microscopy (HAADF-STEM) images were obtained using an FEI Titan Themis aberration-corrected microscope operated at 300 kV and with a probe-corrected cubed Thermo Fisher Scientific Themis Z Microscope operating at 300 kV with a probe semi-convergence angle of 20 rad. Images were processed using Image J.

TEM was conducted by JEM-2100F (JEOL) instrument operating at 200 kV. The samples were sonicated in ethanol and being dropped on the carbon-coated Cu grid before test. The High-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) images were obtained on a Thermo Scientific Themis Z microscope equipped with a probe-forming spherical-aberration corrector.

High-resolution HAADF-STEM images were acquired with a probe-corrected cubed Thermo Fisher Scientific Themis Z Microscope operating at 300 kV with a probe semi-convergence angle of 20.5 mrad. For a quantitative analysis of the HAADF-STEM image, the intensities of the individual atomic columns in a single heterostructure were analyzed by using the StatSTEM software^{48 (link)}. The color code in the intensity map correlates with the total intensity scattered from each atomic column. The intensity is calculated by fitting a Gaussian function to each atomic column: the intensity value of a column equals the volume of its Gaussian peak.

The C/H ratio of the soot samples was determined by an elemental analyser (VARIO EL CUBE) on a dry and ash-free basis.
The carbon structures were characterized by Raman spectroscopy (ThermoFisher DXR), which was carried out by using a He-Ne laser (0.5 mW, 455 nm). The Raman results in the first-order Raman spectrum region were deconvoluted by means of the five-band method^{68 (link)} with the following bands: G (1580 cm⁻¹), D1 (1350 cm⁻¹), D2 (1610 cm⁻¹), D3 (1550 cm⁻¹), and D4 (1180 cm⁻¹). The distributions of different carbon structures of the soot samples are shown in the Supplementary Fig. S4. The integral band area ratio of the D band to G band (I_D1/I_G) was used to quantify the degree of graphitization of soot samples^{69 (link)}.
STEM characterization was performed by means of a ThermoFisher Themis Z microscope equipped with two aberration correctors under 300 kV. HAADF-STEM images were recorded using a convergence semi-angle of 11 mrad and inner and outer collection angles of 59 and 200 mrad, respectively. EDS was carried out using 4 in-column Super-X detectors.

The crystal structure of the samples was examined by X-ray diffraction (XRD, D/max2550V). Raman analysis was carried out by using a Leica DMLM microscope (Renishaw) with the 514 nm laser. SEM characterization was performed using a scanning electron microscope (Hitachi S4800). Aberration-corrected STEM characterization was performed on a Thermo Fisher Themis Z microscope equipped with two aberration correctors under 300 kV. High-angle annular dark-field (HAADF)-STEM images were recorded using a convergence semi-angle of 11 mrad, and inner- and outer collection angles of 59 and 200 mrad, respectively. Energy-dispersive X-ray spectroscopy (EDS) was carried out using 4 in-column Super-X detectors. More detailed chemical compositions were collected on X-ray photoelectron spectroscopy (XPS, Thermo Escalab 250) with Al Kα X-ray beam (1486.6 eV), and all binding energies were calibrated using the C 1 s peak at 284.8 eV as the reference. Inductively coupled plasma optical emission spectroscopy (ICP-OES) was carried out on a NexION 2000-(A-10) to determine the Co concentration. The surface area of the samples was obtained by the method of Brunauer–Emmett–Teller (BET).