The phase purity and crystallinity were characterized by XRD (Bruker D8 Advance DaVinci, Karlsruhe, Germany), powders in Bragg-Brentano setup with a variable slit size, and films using grazing incidence setup with 2° incidence angle. All samples were measured with equal scan conditions, and no data manipulations other than vertical offset were applied. Rietveld refinements were carried out in Bruker AXS Topas version 5. Fundamental parameters peak shape was employed, with starting point in R3c reference unit cell parameters [30 (link)]. Background signal was refined for the most crystalline samples, and fixed to the same value for the remaining samples, where only unit cell parameters and crystallite size were refined. Powder samples were refined by the 2θ range 20°–75°, and films by 21°–49°.
Thermogravimetric analysis combined with mass spectroscopy (TGA-MS, Netzsch STA 449 C and Netzsch QMS 403 C, Selb, Germany) was conducted in synthetic air (20% , 80% ) and argon on dried sols, heating and cooling at 10 °C/min. Scanning electron images were captured on a field emission gun SEM (Zeiss Ultra 55, Limited Edition, Oberkochen, Germany). Fourier transform infrared spectroscopy (FTIR) was done in vacuum by the attenuated total reflectance (ATR) method (Bruker Vertex 80v) on the ground calcined powders.
Thermogravimetric analysis combined with mass spectroscopy (TGA-MS, Netzsch STA 449 C and Netzsch QMS 403 C, Selb, Germany) was conducted in synthetic air (20% , 80% ) and argon on dried sols, heating and cooling at 10 °C/min. Scanning electron images were captured on a field emission gun SEM (Zeiss Ultra 55, Limited Edition, Oberkochen, Germany). Fourier transform infrared spectroscopy (FTIR) was done in vacuum by the attenuated total reflectance (ATR) method (Bruker Vertex 80v) on the ground calcined powders.