Qms 403

The thermal stability of the particles was analyzed with thermogravimetric
analysis (TGA) (Netzsch STA 449 F3 Jupiter & QMS 403 Aëolos
Quadro). The freeze-dried particle powders were loaded in 85 μL
aluminum pans; the loaded amount varied between 7 and 11 mg. The samples
were heated from 40 to 900 °C at a heating rate of 10 °C/min
in the atmosphere of helium gas (50 mL/min).

The obtained materials were characterized by X-ray diffraction (XRD), Fourier transformed infrared (FTIR) spectroscopy, scanning electron microscopy, and differential thermal analysis (DTA). The XRD patterns were obtained using a Miniflex 600 diffractometer with CuKα (λ = 1.5418 Å) radiation (Rigaku, Tokyo, Japan). The patterns of powdered samples were recorded in the range of 2–72°2θ with a 0.05°2θ step. The infrared spectra were collected by KBr pellet method (1 mg sample mixed with 200 mg KBr) with a Nicolet 6700 spectrometer (Thermo Scientific, Waltham, MA, USA). For each measurement, 64 scans were collected in the range of 4000–400 cm⁻¹ and at a 4 cm⁻¹ resolution. The SEM images were obtained using an Quanta 200 FEG microscope under low vacuum (FEI, Hillsboro, OR, USA). The samples were prepared by placing powdered material on a carbon tape. The thermal (DTA/TG) analysis of the samples was carried out using a STA 449F3 instrument coupled with a quadrupole mass spectrometer QMS 403 (Netzsch, Selb, Germany). The measurements were performed using ~20 mg samples in a temperature range of 25–1000 °C (heating rate: 10 °C/min, air atmosphere).