Jsm 6480

The proton NMR spectra were measured at 400 MHz on an NMR spectrometer equipped with Bruker Top Spin 3.2 software (AscendTM 400, Bruker, Madison, WI, USA) using DMSO-d₆ as a solvent at room temperature. FTIR spectra in the range from 600 to 4000 cm⁻¹ were measured on a Fourier transform infrared spectrophotometer (IRAffinity-1S, SHIMADZU, Kyoto, Japan), by placing samples on the surface of a ZnSe crystal using the attenuated total reflectance method. Surface profiles were measured by laser confocal microscopy (VK-9710K, Keyence, Osaka, Japan). The surfaces of the fractured samples were observed by scanning electron microscopy (SEM; JSM-6480, JEOL Ltd., Tokyo, Japan). Thermal stability of polymers, TH-treated CFs, and CF-reinforced composites were evaluated under N₂ atmosphere by elevating the temperature from 23 to 400 °C at the rate of 10 °C/min using a differential thermal thermogravimetry analyzer (DTG-60H, Shimadzu, Japan). The molecular weight was obtained on an ACQUITY APC (Waters Corporation, Milford, MA, USA) equipped with a column (ACQUITY APC XT 2002.5 µm) by flowing a THF solution of a sample at the rate of 0.7 mL/min. After calibrating the column set using polystyrenes with molecular weights ranging from 1220 to 264,000 g/mol, the molecular weight of the sample was measured.

The AgNPs were characterized through UV-Visible spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM) as described by Zhang et al. [12 (link)]. For UV-Vis spectroscopy, AgNP concentration (5 mg/20 ml) was prepared by diluting nanoparticles in deionized water and their absorbance was measured in a wavelength range 300-700 nm to find the wavelength for maximum absorbance. The crystalline size of the AgNPs was measured with an analytical X'Pert, X-ray diffractometer using CuKα1 radiations (λ = 1.540598 Å), at 40 kV and 30 mA. The 2θ range was acquired from 30° to 80°, and JCPDS Cards were used as standards to find the respective phases of the particles. The crystallite size was calculated by using the Debye-Scherrer equation. For SEM images, dried particles were mounted on an aluminum stub and coated with gold to get better contrast. SEM analysis was performed with a scanning electron microscope (JEOL JSM-6480).

Al/(Ti + Al) ratios were determined by energy dispersive X-ray spectroscopy (EDX) in a JEOL JSM-6480 scanning electron microscope with an EDAX Genesis 2000 detection system at 10 kV acceleration voltage.
Three dimensional compositional distributions on the nanometer scale were studied by atom probe tomography (APT) in a CAMECA LEAP 4000X HR. Laser-assisted field evaporation of Ti_0.38Al_0.62N was carried out with a laser energy of 30 pJ and a pulse frequency of 250 kHz. The tip temperature was kept at 60 K. APT specimens were prepared by focused ion beam (FIB) using a FEI HELIOS Nanolab 660 dual-beam microscope employing a standard lift-out procedure^{30 (link)}.

The JEOL JSM-6480 scanning electron microscope made it possible to visualize the surface of the samples after the carbonization process. The operating parameters of the microscope were as follows:

Accelerating voltage: 20 kV;

Working distance: 10 mm;

Mode: SEI;

Magnification: 50×, 200×, 2000×.

SEM micrographs then enabled the determination of the morphology as well as the pore size distribution of the sample surface.

For SEM, the steel plates were briefly rinsed with 0.1 M Hepes buffer (Sigma-Aldrich) at pH 7.2, then fixed in 2.5% glutaraldehyde (Chemi-Teknik AS), 2% paraformaldehyde (VWR, Part of Avantor) and 0.075% Ruthenium Red (Sigma-Aldrich) in 0.1 M Hepes buffer for 4 h at room temperature. Afterwards, the specimens were rinsed in 0.1 M Hepes buffer and then dehydrated through a graded series of ethanol (Antibac AS), (10%, 25%, 50%, 70%), and 90%] for 7 min each and then 3 times in 100% ethanol for 10 min each. After dehydration, the specimens were dried using a chemical hexamethyldisilazane (HMDS) (Sigma-Aldrich), first exchange with 50% solution of HMDS diluted with 100% ethanol for 20 min, then three exchanges with 100% HMDS for 20 min each. Finally, HMDS were removed and the specimens were allowed to air-dry in a fume hood overnight. Dried samples were mounted on stubs using double-sided conductive adhesive carbon tape (both from Chemi-Teknik AS). Specimens were then coated with a 30-nm-thick layer of gold/palladium (Au/Pd) using a sputter coater (polaron) (2.5 kV, 20 mA, 3 min). Specimens were examined with a JSM 6480 (JEOL) scanning electron microscope with digital imaging capabilities. The secondary electron images were collected at an acceleration voltage of 20 kV and digitalized as TIFF computer files.

Scanning electron microscope (SEM) imaging of the µMMN array was performed using JSM 6480 (JEOL, Peabody, MA, USA). For plant tissue imaging, lyophilization of the samples was performed. To obtain a slow freezing rate, the stems were frozen at −12 °C for 24 hours. To prevent the samples from being disturbed when vacuum was introduced, the stems were placed in a freeze-drying container and covered with a polystyrene petri-dish with drilled holes to allow vapor to escape. The container was subsequently connected to a sample valve on the drying chamber of a 1 liter benchtop freeze-dry system (FreeZone, Labconco, Kansas City, Missouri). The samples were dried for 12 hours at a vacuum level of 0.033 mbar with a collector temperature of −40 °C. After 12 hours, the dried samples were removed and ready to be imaged.

The characterization of CeO₂ NPs provides a complete assessment of the morphology, crystalline size, stability, and most importantly functional groups liable to the bioreduction of the synthesized nanoparticles. The CeO₂ NP, CS-CeO₂ nanocomposite morphology was observed by SEM (JEOL, JSM-6480, Tokyo, Japan). The X-ray diffraction of CeO₂ NPs was performed on PANalyticalX’Pert-PRO and interpreted using a matching software. A UV-visible spectrophotometer (Shimadzu, UV-2450, Tokyo, Japan) was utilized to acquire the absorption spectra of CeO₂ NPs. CeO₂ nanoparticles were also evaluated for the existence of biomolecules by Fourier transform infrared spectroscopy (FTIR, Thermo Fischer Scientific, Waltham, MA, USA).