X-ray diffraction (XRD) patterns were collected using a Siemens D-5000 powder X-ray diffractometer operated in Bragg Brentano geometry using Ni-filtered Cu Kα radiation (λ = 0.1541 nm). Data were recorded in the 2θ range 10–80° with an angular step size of 0.026° and a counting time of 1 s per step. The collected data were refined using the Le Bail method by means of the software Rietica [34 (link),35 (link)]. Raman spectra were collected from powder samples onto a glass slide as substrate, with a Renishaw in Via Reflex Raman microscope (Renishaw, Gloucestershire, UK). Experiments were conducted at room temperature using 532 and 633 nm excitation wavelengths. Field emission scanning electron microscopy (FESEM) was conducted on a JEOL JSM-6700 F. Samples for transmission electron microscopy (TEM) studies were prepared by dropping a diluted suspension of the samples onto ultra-thin carbon-coated copper grids. Imaging was performed on a JEOL JEM 1010 instrument operated at 100 kV and equipped with a CCD camera (JEOL, Tokyo, Japan).
Via reflex raman microscope
Manufactured by Renishaw
Sourced in United Kingdom
The Via Reflex Raman Microscope is a versatile analytical instrument designed for Raman spectroscopy. It features a high-performance optical system and advanced imaging capabilities, enabling the characterization and analysis of materials at the micro-scale. The core function of the Via Reflex Raman Microscope is to provide non-destructive, label-free chemical and structural analysis of samples.
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3 protocols using via reflex raman microscope
1
Structural Characterization of Materials
2
Raman Scattering Spectroscopy of Liquid Samples
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Raman scattering spectra of the liquid samples placed onto a quartz plate (identical conditions as in the FTIR experiments) were recorded with the Via Reflex Raman Microscope from Renishaw (Wotton-under-Edge, UK), equipped with two holographic ultrahigh precision diffraction grating stages and a high sensitivity ultralow noise CCD detector. A 514.5 nm Ar+ ion laser was used to record Raman scattering. The spectra were accumulated within a 10 s integration time.
3
Micro Raman Spectroscopy Characterization
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Samples were evaluated by a micro Raman spectroscopy system (in Via Reflex Raman Microscope, Renishaw). The excitation light source was a continuous-wave laser diode with 785-nm wavelength (NIR, Renishaw). The laser light was focused on the sample surface by an objective lens (Plan Apo ×50, Leica). The focal spot of the laser beam was about 2 μm in diameter. Raman scatterings were collected by the same objective lens and passed through Rayleigh filters. Raman spectra were acquired by a single spectrometer, whose focal length and diffraction grating groove density were 250 mm and 1800 line/mm, respectively, which provided a spectral resolution of 2 cm -1 . Samples were under atmosphere pressure at room temperature. We took 49 spectra for each sample at different positions in a 350 × 350 μm area so as to compensate for any position variability. Nine deviated spectra were removed, and the 40 remaining spectra were averaged to obtain the spectrum for each sample. All Raman spectra were taken in 30 s from 10 to 2000 cm -1 .
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