X pert diffractometer

The purity of MFM-300(V^III) was confirmed by powder X-ray diffraction before loading into the MMM. The membrane morphology was studied by scanning electron microscopy (SEM) using a Hitachi S-4800 Field-Emission Scanning Electron Microscope with Energy Dispersive X-ray (EDX) detector and cold cathode electron source. The membrane cross section was prepared via freeze fracturing using liquid N₂. The sample was then coated with gold via sputtering using an Emitech coater. PXRD analysis was also carried out on a Philips X'Pert diffractometer to ensure retention of the crystallinity of the MOF once incorporated into the membrane.

XRPD was used for characterizing crystalline materials and providing information on structures. The dust and surface sweep method were used. Approximately 20 mg of sample was dispersed on a sample holder and loaded into a Philips X’PERT^® diffractometer equipment. Each sample was exposed to Cu-kα radiation, the angles of incidence being from 5° to 50°. The test conditions are 40 mV voltage and 55 mA intensity. The diffractograms obtained from the raw materials (MLX, lactose, Metolose^® and Eudragit^®) and the CNM formulation and its placebo make it possible to know if the samples are crystalline or amorphous. GID method has also been used, which consists in that the angle of incidence (θ) remains fixed while the detector moves normally around the axis of the goniometer [38 (link)]. GID is a surface-sensitive technique that, allows the characterization of epitaxial films with thicknesses down to a few atomic layers. All measurements were made with a Philips X’PERT^® diffractometer, where the radiation was the same as for the measurements by the powder method. In this study, we have used an incidence angle (θ) of 1°. Before the measurements, the equipment was carefully aligned and calibrated. A spatial sample holder was used that could be adjusted to the height of the sample. Under these conditions, the CNM formulation was measured.

SnO₂ nanoparticles were analyzed by X-ray diffraction (XRD) performed on a Philips X’Pert diffractometer (2θ from 20° to 80°, λ = 1.5406 Å) with Cu Kα radiation. Micromorphology and element distribution of pure SnO₂ and Pt-decorated SnO₂ were characterized by field emission scanning electron microscopy (FE-SEM, Hitachi S-4800, Tokyo, Japan) and an energy dispersive spectrometer (EDS, Hitachi S-4800, Tokyo, Japan). TEM images were obtained by a JEOL 2100F microscope (Tokyo, Japan). The X-ray photoelectron spectroscopy (XPS) test was conducted by a Kratos XSAM800 spectrometer (Manchester, England).

X-ray powder diffraction (XRD) patterns were acquired on a PHILIPS X’PERT diffractometer using Cu Kα radiation. The data were recorded from 5° to 50° (2θ) with a resolution of 0.01°. Scanning electron microscopy (SEM) micrographs were obtained on a XL30 ESEM (Philips, Lelyweg, the Netherlands) electronic microscope operating at 200 kV. Nitrogen adsorption–desorption isotherms at −196 °C were measured using an AutoSorb equipment (Quantachrome Instruments, Boynton Beach, Florida, USA). Samples were degassed at 150 °C and high vacuum during 180 h. The micropore surface area was calculated by using the Brunauer–Emmett–Teller (BET) model [37 (link)]. The pore volume and diameter were estimated by non-local DFT calculations, assuming a kernel model of N₂ at −196 °C on carbon (cylindrical pores, NL-DFT equilibrium model) [38 (link)] and external surface was estimated by t-plot method and Harkins Jura equation [39 (link)]. Simultaneous thermogravimetry and derivative thermogravimetric analyses (TGA/DTG) were carried out under a nitrogen atmosphere with an N₂ flow of 100 mL·min⁻¹ at a heating rate of 5 °C/min up to 700 °C, using a SDT 2860 apparatus (TA Instruments, New Castle, DE, USA).

The phase composition of the as-prepared powders was analyzed by powder X-ray diffraction (XRD) analyses (Philips X’ Pert diffractometer) with CuKα radiation. Environmental scanning electron microscopy (ESEM, Helios Nanolab 600i) and high-resolution transmission electron microscopy (HRTEM JEM-2100) were used to observe the morphology of the graphene sheets. The TEM specimens were prepared by dropping ethanol/water (38 v/v%) solution containing 1 wt % N-doped graphene onto a copper grid and drying at 100 °C. Raman spectra were obtained using a Raman Station (B&WTEK, BWS435-532SY) with a 532 nm wavelength laser corresponding to 2.34 eV, 30% of the laser power (total power: 240 mW) was used on the samples. X-ray photoelectron spectroscopy (XPS, Thermo Fisher) was utilized to determine the bonding characteristics of the samples. All XPS peaks are calibrated according to the C 1 s peak (284.6 eV). The composition was confirmed using X-ray fluorescence (XRF, AXIOS-PW4400) in order to determine the presence of any metallic elements. 2 milligrams of N-doped graphene powder was spread out on the surface of boric acid powder (99.0%, Sinopharm Chemical Reagent Co., Ltd.), the effective test zone is a disk surface with a diameter of 20 mm. The magnetic properties were measured using a Quantum Design MPMS magnetometer based on a superconducting quantum interference device (SQUID).