Asap 2420 sorptometer

X-ray Diffraction (XRD) Patterns of the samples were obtained with a Philips X’PERT diffractometer using Cu Kα radiation. Nitrogen adsorption-desorption isotherms were measured at −196 °C using the micrometrics ASAP 2420 sorptometer to determine textural properties. All samples were degassed at 350 °C for 16 h. The total pore volume was determined from the amount of nitrogen adsorbed at a relative pressure of 0.97. Pore size distributions were determined from the adsorption branches of isotherms using the DFT model with cylindrical geometry of the pores. Transmission electron microscopy (TEM) micrographs were taken using a JEOL 2100F electron microscope operating at 200 kV. The samples for TEM analysis were prepared by suspending a small amount of solid in ethanol. A drop of this suspension was then dispersed onto a holey carbon film on a copper grid, followed by drying at room temperature. The morphology was evaluated by scanning electron microscopy (SEM) with an FE-SEM FEI Nova NanoSEM 230 microscope with vCD detector using chromium coating.

Powder X-Ray Diffraction (PXRD) patterns were collected in an X-Ray Polycrystalline X'Pert Pro PANalytical diffractometer using CuK_α radiation (λ = 1.5406 Å), with accelerating voltage and current of 45 kV and 40 mA, respectively. N₂ adsorption measurements were conducted at −196°C using a Micrometrics ASAP 2420 sorptometer to determine textural properties. All samples were pre-treated at 150°C for 16 h. Pore size distributions were determined from the adsorption branches of isotherms, using the Barrett-Joyner-Halenda (BJH) following the Kruk-Jaroniec-Sayari model. Scanning electron microscopy and EDX analyses were carried out on a Hitachi TM1000 microscope equipped with EDX detector. Samples were observed without coating. Scanning transmission electron microscopy (STEM) analyses were performed in a cold FEG JEOL GrandARM 300 operated at 300 kV. The microscope is equipped with a double spherical aberration corrector from JEOL. The spatial resolution at 300 kV was 0.7 Å. The microscope is also fitted with a JEOL EDS system and a Gatan Quantum Energy Filter. Typically, the beam current employed was set between 1 and 2 pA, with a total exposure time of 6 s. In prior observation, the samples were crushed using mortar and pestle for 3 min, suspended in ethanol and sonicated. A few drops of the suspension were placed onto holey carbon copper grids.