The surface morphology and elemental composition analysis of the substrates were monitored using a field emission scanning electron microscopy (FE-SEM, JEOL, JSM-7001FA). The chemical properties analysis was performed using X-ray diffraction (XRD, Rigaku, Tokyo, Japan, RINT2500HLB) with a Cu Kα line of 1.5406 Å and a scanning field of 2.5° ≦ 2θ ≦ 100°. Peak fitting was performed in referenced to JCPDS card 4-0831 and 5-0664. TEM micrographs, SAED patterns and HRTEM micrographs for the NCs were obtained using a double Cs-corrected-TEM (FEI, Titan cubed) operated at 300 kV.
Titan cubed
Manufactured by Thermo Fisher Scientific
The Titan Cubed is a versatile laboratory equipment designed for high-performance sample processing. It features a compact and robust construction, enabling efficient and reliable operation within the laboratory environment.
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5 protocols using titan cubed
1
Comprehensive Substrate Characterization
2
Structural Analysis of Sodium Ruthenium Oxides
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The synchrotron XRD patterns were recorded at Aichi Synchrotron Radiation Center (Aichi-SR, O3-Na2RuO3), and Photon Factory at High Energy Accelerator Research organization (KEK-PF, BL-8B) or SPring-8 (O1-Na1RuO3 and O1′-Na1/2RuO3, beamline 02B2). All samples were protected from air exposure during the measurement. Rietveld refinement was performed using Jana200634 . Analyses of the stacking faults in the materials were carried out using the FAULTS software27 (link). The crystal structures were drawn using VESTA35 (link). Selected Area Electron Diffraction (SAED) patterns were recorded using an electron microscope (HF-3000S; Hitachi Ltd. and Titan Cubed; FEI Co.) operated at 300 kV. The camera length for SAED was calibrated with a Si crystal.
3
In-situ X-ray Characterization of Samples
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Ex situ X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS) measurements were performed on samples without exposure to air at BL07LSU of SPring‐8. A bulk‐sensitive partial fluorescence yield (PFY) mode was employed for O K‐edge XAS. Extended X-ray absorption fine structure was conducted at the BL-9C Beamline of the Photon Factroy, KEK, Japan. SAED patterns were recorded using an electron microscope (Titan Cubed, FEI Co.) operated at 80 kV after transferring the samples without exposure to air.
4
Graphene Nanoplatelets Characterization
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The milled samples, i.e., GNPs were confirmed by HRTEM observation as well as X-ray diffraction pattern analysis. The GNPs including metal particles originated from the steel balls were purified through a solution treatment where the samples are dispersed in ethyl alcohol with sonication and the metal impurities are removed by magnets. HRTEM observation for grown graphene sheets were performed by a JEM-2100F operating at 200 kV and a FEI Titan Cubed with aberration corrector and a monochrometer operating at 80 kV. Raman analysis was performed by a Renishaw In-Via Raman Microscope with laser excitation of 532 nm and spot size of 1–2 μm.
5
Atomic-Scale Imaging of 2D Materials
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A chemical-vapor-deposited graphene (TEM2000GL, ALLIANCE Biosystems), which was transferred onto a Cu mesh without a supporting film, was used as a graphene specimen. Solutions of WS2 and MoS2 (Graphene Supermarket) were dispersed on holey carbon films.
Experimental ADF images were obtained using an aberration-corrected STEM instrument (FEI, Titan cubed) at an acceleration voltage of 80 kV. An ADF detector (E.A. Fischione Instruments, Inc., Model 3000) and analog-digital (AD) converter (Gatan, DigiScan II) were used to acquire the ADF images. The ADF images are processed using software (Gatan, DigitalMicrograph), in which the nonlinear responses of the ADF detector and AD converter were corrected using an empirical function. The incident probe current was 20 pA, which was measured using a charge-coupled device (CCD) camera whose sensitivity was calibrated in advance. The ADF angle range should be carefully evaluated31 (link),32 (link) and our procedure was given in the Supplementary Information.
To avoid contamination during observations, STEM specimens were annealed in vacuum at 523 K before STEM observations. The specimen temperature during the STEM observations was room temperature for graphene and 873 K for MoS2 and WS2. A specimen heating holder (Protochips, Aduro) was used for the MoS2 and WS2 specimens.
Experimental ADF images were obtained using an aberration-corrected STEM instrument (FEI, Titan cubed) at an acceleration voltage of 80 kV. An ADF detector (E.A. Fischione Instruments, Inc., Model 3000) and analog-digital (AD) converter (Gatan, DigiScan II) were used to acquire the ADF images. The ADF images are processed using software (Gatan, DigitalMicrograph), in which the nonlinear responses of the ADF detector and AD converter were corrected using an empirical function. The incident probe current was 20 pA, which was measured using a charge-coupled device (CCD) camera whose sensitivity was calibrated in advance. The ADF angle range should be carefully evaluated31 (link),32 (link) and our procedure was given in the Supplementary Information.
To avoid contamination during observations, STEM specimens were annealed in vacuum at 523 K before STEM observations. The specimen temperature during the STEM observations was room temperature for graphene and 873 K for MoS2 and WS2. A specimen heating holder (Protochips, Aduro) was used for the MoS2 and WS2 specimens.
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