Synthesis of aluminium borate-boron oxide and binary titanium-boron and zirconium-boron oxides from metal alkoxides and (MeO)3B3O3 in non-aqueous solvents

The reaction of metal alkoxides M(OR)4 (M = Ti, Zr; R = organyl) with (MeO)3B3O3 (1 : 0.67) in dry propan-2-one at room temperature led to gels which when dried and calcined in air for 24 h at 500-1000 degrees C afforded bi-phased mixed-oxide materials formulated as 4TiO2 x 3B2O3 and ZrO2 x B2O3 in high ceramic yields and purity; the B2O3 phases of these materials were amorphous. The materials remained amorphous upon calcination at lower temperatures. The TiO2 phase of the 4TiO2 x 3B2O3 was crystalline when calcined at higher temperatures with either anatase (600 degrees C) or rutile (>800 degrees C) being obtained. The ZrO2 phase of the ZrO2 x B2O3 was crystalline when calcined at higher temperatures and was obtained as a metastable tetragonal phase (<700 degrees C) or baddeleylite (>800 degrees C). In a similar reaction, Al(O(i)Pr)3 (2 : 1) gave a bi-phased aluminium borate-boron oxide (Al18B4O(33).7B2O3) after calcination at >700 degrees C. The dried gels and oxide materials were all characterized by elemental analysis, TGA-DSC, and powder XRD.