Synthesis of TiO2 nanopartlices by sol-gel method : bachelor thesis

Istraživanja u ovom radu usmjerena su na sol-gel sintezu nanostrukturiranih čestica TiO 2 te karakterizaciju istih. Kao izvor titana korišten je titanijev n-butoksid ( Ti[O(CH 2 ) 3 CH 3 ] 4 ), a kao otapalo 96%-tni etanol odnosno apsolutni etanol uz dodatak HCl odnosno HNO 3 . Sinteze su provedene pri sobnoj temperaturi uz konstantno miješanje u trajanju od 4 sata. Kruta faza iz pripravljenih suspenzija je separirana od tekuće faze i osušena pri temperaturi od 80°C u trajanju od 1 odnosno 2 sata. Osušeni prah je zatim kalciniran pri temperaturi od 450°C u trajanju od 3 sata. Pripravljeni uzorci su karakterizirani difrakcijom rendgenskih zraka na polikristalnim uzorcima (XRD), infracrvenom spektroskopijom s Fourierovom transformacijom (FT-IR) te pretražnom elektronskom mikroskopijom (SEM). Rezultati istraživanja ukazuju da nakon provedenog sušenja pri 80 o C u uzorku D dolazi do kristalizacije strukturno uređenog TiO 2 u formi anatasa, u ostalim uzorcima produkt sol-gel reakcije je produkt koji nema strukturnu uređenost dugog dosega što ukazuje na amorfnu strukturu materijala. Nakon provedene kalcinacije pri 450 o C u trajanju od 3 sata u uzorku D dolazi do kristalizacije dvije strukturno uređene forme TiO 2 i to anatasa i brukita dok u ostalim uzorcima kristalizira čisti TiO 2 u formi anatasa.Research in this work is focused on sol-gel synthesis of nanostructured TiO 2 particles and their characterization. Titanium n-butoxide ( Ti[O(CH 2 ) 3 CH 3 ] 4 ) was used as a source of titanium, and 96% ethanol or absolute ethanol with the addition of HCl or HNO 3 . The syntheses were carried out at room temperature with constant stirring for 4 hours. Solid phase from the obtained milky suspension were separated and dried at a temperature of 80°C for 1 or 2 hours. The dried powder was then calcined at a temperature of 450°C for 3 hours. The prepared samples were characterized by X-ray diffraction on polycrystalline samples (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). The research results indicate that after drying at 80 o C in sample D, have a structurally ordered phase of TiO 2 which crystallizes in the form of anatase, in other samples the product of the sol-gel reaction is a product which does not have a long-range structural order, what suggest on the amorphous structure. After calcination at 450 o C for 3 hours in sample D, two structurally ordered forms of TiO 2 crystallize, namely anatase and brookite, while pure TiO 2 crystallizes in the form of anatase in the other sample