Titan cubed themis g2 300

The PXRD results of MIL-101 crystals were obtained using a diffractometer (Rigaku D/Max-RB) with the CuKα radiation at 40 kV and 120 mA. The SEM images were obtained under a high-resolution SEM (JEOL, JSM-7401) at 1 kV. The ADF-STEM images were also obtained under the Cs-corrected STEM (FEI Titan Cubed Themis G2 300) operated at 300 kV with the same convergence semi-angle, collection angle and aberration coefficients as those in iDPC-STEM imaging. The electron-beam current of ADF-STEM was set as 0.7 ~ 3.2 pA.

N₂ adsorption analysis was conducted on a Quantachrome Autosorb IQ instrument. All powder samples were degassed at 150 °C overnight prior to actual measurement. The surface area was calculated by using BET calculations. The pore size distribution (PSD) plot was recorded from the adsorption branch of the isotherm based on the QSDFT model for slit/cylinder pores. XPS were obtained by using an XPS device (ESCAL 250) to detect the compositions of the M-Art M and analyzed by Avantage to confirm the successful introduction of the metals. SEM images were obtained by using an Apreo S HiVoc (Thermo Fisher Scientific, FEI). Cryo-SEM images were obtained by using Quanta 450FEG (FEI Ltd., USA). TEM images and EDS mapping were obtained via a Talos F200x TEM microscope (FEI Ltd., USA) operated at 200 kV and analyzed by GMS-freeanalysis. XRD pattern presented the crystal phase state via a Bruker D8 Focus X-ray diffractometer and analyzed by MDI Jade and Origin. The X-ray absorption spectra were collected on the beamline BL07A1 in NSRRC and the radiation was monochromatized by a Si (111) double-crystal monochromator. XANES and EXAFS data reduction and analysis were handled via Athena software. Cs-corrected (S)TEM (FEI Titan Cubed Themis G2 300) was used for high-resolution HAADF-STEM.

The iDPC-STEM imaging was conducted using a Cs-corrected (S)TEM (FEI Titan Cubed Themis G2 300). The operating voltage is 300 kV. The instrument is equipped with a DCOR+ spherical aberration corrector for the scanning probe that is aligned by a standard gold sample before imaging. The following aberration coefficients were used: A1 = 1.47 nm; A2 = 6.07 nm; B2 = 5.4 nm; C3 = −91.2 nm; A3 = 225 nm; S3 = 66.6 nm; A4 = 1.57 µm, D4 = 2.24 µm, B4 = 2.3 µm, C5 = 615 µm, A5 = 170 µm, S5 = 34 µm, and R5 = 34 µm, assuring a 60 pm resolution under a convergence semi-angle of 23.6 mrad. The convergence semi-angle for the iDPC-STEM is 15 mrad. The collection angle for the iDPC-STEM is 5–26 mrad. The beam current can be measured by the Faraday cup. The used beam current for the iDPC-STEM imaging is lower than 0.1 pA (measurement limit of beam current by the Faraday cup). Then, the corresponding dwell time of probe scanning is 32 μs/pixel with the pixel size of 0.1257 Å. Based on the beam current, dwell time, and pixel size, the calculated dose is <1266 e⁻/Ų.

Raman spectra were recorded on a DXRxi Raman spectrometer with a 532 nm excitation wavelength. ASAP 2020 Accelerated Surface Area and Porosimetry System was used to measure the specific surface area and pores size distribution. XPS measurements were taken on an Axis Supra spectrometer (Kratos Analytical Ltd.). The microscopic observations were characterized by field‐emission scanning electron microscope (S4800, Hitachi), TEM (JEM‐2100F, JEOL) and spherical aberration‐corrected TEM (Titan Cubed Themis G2 300, FEI). Cryo‐TEM characterizations were performed on JEM‐2100F cryo‐TEM and operated at 200 kV, in which the ALi‐HDGs samples and cryo‐TEM test temperatures were kept at about −176 °C by the liquid nitrogen. ALi‐HDGs samples onto the cryo‐TEM holder were placed in the Ar‐filled glovebox, and then sealed by a shutter in the air‐insulated tube to prevent the air exposure. The schematic illustration of the details to prepare and transfer the samples into cryo‐TEM is shown in Figure S27, Supporting Information.

A PPC/PDMS stamp was used to pick the ReS₂ flakes from the substrates, and was covered onto the SiN_x grids using a transfer stage. The temperature was raised to 110 °C until the stamps and the grids were well contacted, and then the grids and the stamps were placed in acetone for 24 h at room temperature to remove the PPC. STEM-ADF images were taken using FEI Titan Cubed Themis G2 300 operated at 300 kV. The convergence semi-angle was 21.3 mrad while the collection angle of ADF detector was 39–200 mrad. While acquiring images, the probe current was ~8 pA, and the dwell time was 2 μs/pixel. For this condition, the radiation damages can be avoided and images with high signal-to-noise ratio were obtained.

The in‐situ HADDF‐STEM experiments were performed on an aberration‐corrected STEM (FEI Titan Cubed Themis G2 300) equipped with Cs double corrector DCOR and a high‐brightness field emission gun (X‐FEG), which was operated at an acceleration voltage of 300 kV. The sample obtained by pyrolysis of Co/Zn‐ZIF at 850 °C and used for the above ETEM experiment was heated with the beam off to 1000 °C in Cs‐STEM at a rate of 1 °C s⁻¹ under high vacuum. The STEM images were then taken with the beam on.

Transmission electron microscopy (TEM, FEI Tecnai G² F20, Hillsboro, Oregon, USA, operated at 200 kV) was used to characterize the microstructure of the SWCNTs and SWCNT@h-BN films. High-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) image and electron energy loss spectroscopy (EELS) mapping of SWCNT@h-BN were acquired using a spherical aberration-corrected TEM (FEI Titan Cubed Themis G2300, Hillsboro, Oregon, USA, operated at 300 kV).
The Raman spectra of SWCNTs and SWCNT@h-BN films were collected by micro-Raman spectroscopy (Witec, ALPHA300R, Ulm, Baden-Württemberg Germany, equipped with 532 and 633 nm lasers). The ratios of I_G/I_D ratio were randomly collected from five points for each sample and calculated by averaging these data. Fourier transform infrared (FT-IR) spectra of all samples were collected from spectrometer (Bruker Tensor 27, Karlsruhe, Baden-Württemberg, Germany) in the range of 400–4000 cm⁻¹. X-ray photoelectron spectroscopy (XPS, ESCALABXi+, Waltham, MA, USA, operated at 15 kV and 150 W) was used to analyze the chemical composition of surface layers using a pass energy of 50 eV with an energy step size of 0.1 eV. The collected spectra were calibrated by the standard C 1s peak located at 284.6 eV.