Preparation of titania from tetrakis(diethylamino)titanium via hydrolysis

The conversion of tetrakis(diethylamino)titanium (Ti(NEt2)(4)) into titania via either a combination of hydrolysis (Ti(NEt2)(4) : THF : H2O = 1 : 10 : x, x = 2, 4, 10) at ambient conditions and calcination (method A) or hydro lysis in a water-tetrahydrofuran (THF) mixture (Ti(NEt2)(4) : THF : H2O = 1 : 10 : 100) at reflux (method B) was investigated. Titanium tertiary butox ide (Ti((OBu)-Bu-t)(4)) was also used as a substitute for Ti(NEt2)(4). The hydrolysis via method A resulted in the formation of amorphous solids conta ining organics. Thermal analyses showed that the hydrolysis products showed mass losses up to 500 degreesC probably due to the presence of diethylamin e (Et2NH) formed via the hydrolysis of Ti(NEt2)(4) in the hydrolysis produc ts, while a mass loss of the hydrolysis product from Ti((OBu)-Bu-t)(4) was completed up to about 200 degreesC. After calcination at greater than or eq ual to 600 degreesC, anatase or a mixture of anatase and rutile was obtaine d. The crystallization behavior of the hydrolysis products from Ti(NEt2)(4) was different from that of the hydrolysis product from Ti((OBu)-Bu-t)(4). The hydrolysis via method B gave only an amorphous material from Ti(NEt2)(4 ), while a crystalline titania (anatase and brookite) formed from Ti((OBu)- Bu-t)(4).