The scanning electron microscope (SEM) and transmission electron microscopy (TEM) images were obtained with the NTC JSM-6390LV SEM system and Hitachi H-7650 TEM system, respectively. The X-ray diffraction (XRD) analysis was conducted on the Rigaku Miniflex 600 system. The solution in 96-well ELISA plates for the absorbance determination was performed with the SpectraMax i3 multifunctional system.
Miniflex 600 system
Manufactured by Rigaku
Sourced in Japan
The Miniflex 600 system is a compact, versatile X-ray diffractometer designed for a wide range of applications. It features a 600 W X-ray source, a goniometer with a minimum step size of 0.001°, and a high-speed semiconductor detector. The Miniflex 600 system is capable of performing qualitative and quantitative phase analysis, thin-film analysis, and other X-ray diffraction measurements.
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3 protocols using miniflex 600 system
1
Characterization of Nanomaterials using Advanced Microscopy and Spectroscopy
2
Nanoscale Characterization of CeO2 and TM@CeO2 NPs
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The morphology of CeO2, Cr@CeO2, and Fe@CeO2 NPs was analyzed by HRTEM (JEM-ARM200CF, JEOL Ltd., Tokyo, Japan) using an accelerating voltage of 200 kV. In addition, the distribution of the constituent elements within the NPs at the nanoscale was mapped using STEM-EDS (JED-2300T, JEOL Ltd., Japan). The XRD data were recorded in the range 20–100° in a scanning step of 0.02° for 0.3 s using a MiniFlex600 system (Rigaku, Tokyo, Japan) with Cu Kα radiation operated at 15 mA and 40 kV. Crystallite sizes and lattice parameters were calculated by Pawley refinement of the corresponding diffraction patterns using TOPAS software (Version 4.2, Bruker, Rheinstetten, Germany). Raman spectra were obtained using an XploRA Raman spectrometer (HORIBA, Kyoto, Japan) with a diode-pumped solid-state laser of 532 nm wavelength operating at 10 mW. The UV-Vis DRS experiments were performed on a UV-2600i UV-Vis spectrophotometer (Shimadzu, Kyoto, Japan) equipped with integrated spheres. To compare the electronic structure of CeO2 and TM@CeO2 NPs, we obtained Ce M-edge, O K-edge, Cr L-edge, and Fe L-edge spectra using XAS in the 8A1 beamline at the Pohang Accelerator Laboratory with a PHI-3057 electron analyzer (Physical Electronics, Chanhassen, MN, USA) under the base pressure of 2.0 × 10−9 Torr.
3
Powder X-ray Diffraction Analysis
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For PXRD measurements, solution-processed
samples were dried overnight under vacuum and then ground into powdered
forms. PXRD measurements were carried out on a Rigaku MiniFlex600
system equipped with a D/teX detector using a Ni-filtered Cu Kα
radiation source. Typical PXRD scans were performed in the 5°–90°
(2θ) range, with a step size of 0.02° to determine phase
identity and purity. Data analysis was performed using the Rigaku’s
PDXL2 software package. The baseline originating from the glass slides
used to collect data was corrected using the embedded tool in the
PDXL2 software, and the data were fitted using the decomposition method
(also known as Pawley fitting) embedded in the PDXL2 software package.
samples were dried overnight under vacuum and then ground into powdered
forms. PXRD measurements were carried out on a Rigaku MiniFlex600
system equipped with a D/teX detector using a Ni-filtered Cu Kα
radiation source. Typical PXRD scans were performed in the 5°–90°
(2θ) range, with a step size of 0.02° to determine phase
identity and purity. Data analysis was performed using the Rigaku’s
PDXL2 software package. The baseline originating from the glass slides
used to collect data was corrected using the embedded tool in the
PDXL2 software, and the data were fitted using the decomposition method
(also known as Pawley fitting) embedded in the PDXL2 software package.
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