PXRD patterns were collected using PANalytical Aeris benchtop powder diffractometer (CuKα radiation with Ni filter; λ= 1.5418 Å, 45 kV, 40 mA) in Bragg-Brentano geometry in a 5°-50° 2θ range (0.025° step). Particle size distribution (PSD) curves were obtained by laser light scattering analysis using Malvern Mastersizer 2000 laser light scattering granulometry. The samples were exposed to ultrasonication during the measurement. Scanning electron microscopy (SEM) images were acquired on a Jeol JSM 7000F scanning electron microscope and a MIRA-LMH (TESCAN) scanning electron microscope equipped with a field emission gun. Solid-state nuclear magnetic resonance spectroscopy measurements were performed on a 600 MHz Varian spectrometer, using 3.2 mm HX CPMAS probe to obtain 27Al MAS, 29Si MAS and 1H-29Si CPMAS spectra. All of the samples were measured under magic-angle spinning frequency of 20 kHz. Operating Larmor frequencies for 1H, 27Al, and 29Si nuclei were 599.34 MHz, 156.17 MHz and 119.06 MHz, respectively. To obtain directly detected 27Al and 29Si MAS spectra a single pulse of 1.0 µs with recycle delay of 0.1 s and a single pulse of 2.8 µs with recycle delay of 60 s was used, respectively. In the case of 1H-29Si CPMAS measurements, a single pulse of 2.85 µs was used to excite 1H nuclei with a following contact time of 5.0 ms to transfer the polarization to 29Si nuclei, recycle delay was 1.0 s. NMR spectra were deconvoluted using dmfit software. Transmission electron microscopy (TEM) analysis was carried out on a FEI Talos F200X microscope operated at 200 kV. The samples were measured with high-resolution TEM (HRTEM), fast Fourier transform (FFT), and electron diffraction (ED) techniques. Chemical composition of selected samples was assessed on the grounds of results obtained by a PerkinElmer AAnalyst 200 atomic absorption spectrometer. The N2 physisorption isotherms were measured at −196 °C utilizing Micromeritics 3Flex high resolution volumetric adsorption analyser. About 100 mg of the sample was degassed at 300 °C under vacuum overnight prior to the analysis. Micropore volume (Vmic) was evaluated on the grounds of the t-plot method, and total pore volume (Vtot) was determined by the amount of adsorbed nitrogen at p/p0 = 0.95. Mesopore volume (Vmeso) is defined as Vtot - Vmic. Raman spectra of the powder samples were collected employing Maya2000 Pro spectrometer in Raman spectroscopy mode using red laser (785 nm). The interval time for each scan was set to 5000 ms, and the number of scans per interval was 80 at a laser power of 60 mW. Each sample was put on a thin glass slice and levelled with a spatula to ensure surface flatness.