The phase and the crystalline structure of the products were characterized by X-ray powder diffraction (XRD, a Philips X’ pert PRO MPD diffractometer) with Cu Kα radiation (λ = 0.15406 nm). The size and morphology of samples were monitored using a Zeiss Supra 55 field scanning electron microscope (SEM) operating in high vacuum mode with an acceleration voltage of 15 kV. TEM, HRTEM, STEM and elemental mapping by EDS analysis were performed by a FEI Tecnai F20 transmission electron microscope with an accelerating voltage of 200 kV. The ultraviolet-visible (UV-vis) absorption spectrum was recorded by a Thermo Scientific Evolution 220 Diode Array Spectrophotometer. Raman spectra were measured with an HR 800 Raman spectrometer (J Y, France) equipped with a synapse CCD detector and a confocal Olympus microscope. The spectrograph was operated with 600 g/mm gratings and a 633 nm He-Ne laser was applied for excitation. SERS spectra were collected by an objective with a magnification of x50 (Olympus) with a numerical aperture of 0.90 and an accumulation time of 1 s. SERS experiments were conducted in the line mapping mode with 1 μm increments using 1 × 10−7 M R6G water solution.
Supra 55 field
Manufactured by Zeiss
The Supra 55 field is a high-performance scanning electron microscope (SEM) designed for a wide range of applications. It features a high-resolution field emission gun (FEG) and advanced imaging capabilities, providing detailed analysis of samples at the nanoscale level.
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3 protocols using supra 55 field
1
Comprehensive Materials Characterization Protocol
2
Characterization of Graphene Nanowires
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Xplora Raman Spectroscope was used to measure the Raman spectra of the GNWs with a 532 nm line of the semiconductor laser. A Zeiss Supra 55 field emission scanning electron microscope (SEM) was used to observe the surface morphology of the synthesized GNWs. The optical transmittance of GNWs was measured by UV-Vis-NIR spectrometer (UV-2600) in the wavelength range from 300 to 1400 nm. The electrical properties of the GNWs were measured by the Hall effect measurement system (HMS 5000). High-resolution transmission electron microscopy (HRTEM) images were taken on a JEOL 2100 TEM microscope operated at 300 kV. The thickness of HfO2 was measured using a profilometer (Bruker, DektakXT-A). The surface roughness of GNWs was characterized by S600LS atomic force microscope (AFM). The capacitance–voltage (C–V) of the fabricated Al/HfO2/p-Si metal–oxide–semiconductor (MOS) capacitor was measured using a Keithley 4200 semiconductor parameter analyzer. The current–voltage (I–V) characteristics of the fabricated photodetectors were measured by Keithley 4200 source meter. Illumination was generated using a light-emitting diode (LED) with a beam diameter of 4 mm and a spectral wavelength of 532 nm in air.
3
Characterization of As-Cast Alloy Microstructure
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Phase identification of the as-cast alloys was conducted by XRD with Cu Kα radiation (MXP21VAHF). Microstructure was characterized by a Zeiss Supra 55 field emission scanning electron microscope equipped with an AZtecHKL EBSD (electron backscattering patterns) system. EBSD specimens were initially polished to 2000-grit SiC paper and subsequently electrochemically polished for the final surface clarification. The polishing was using a 6% perchloric acid + 30% n-butyl alcohol + 64% methyl alcohol solution with a direct voltage of 30 V at room temperature. An aberration-corrected FEI Titan G260-300 kV scanning transmission electron microscope was used to analyze the atomic structure of the as-cast samples. The TEM specimens were first mechanically ground to 50-μm thickness and then twin-jet electropolished using 6% perchloric acid + 30% n-butyl alcohol + 64% methyl alcohol solution. The specimens for the atom probe tomography measurements were prepared by focused ion beam milling on a dual-beam Helios 600. The CAMECA integrated visualization and analysis software IVAS 3.8.4 was used for data processing and three-dimensional atomic reconstruction.
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