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

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Abstract
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 °C afforded bi-phased mixed-oxide materials formulated as 4TiO2·3B2O3 and ZrO2·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 4TiO2·3B2O3 was crystalline when calcined at higher temperatures with either anatase (600 °C) or rutile (>800 °C) being obtained. The ZrO2 phase of the ZrO2·B2O3 was crystalline when calcined at higher temperatures and was obtained as a metastable tetragonal phase (800 °C). In a similar reaction, Al(OiPr)3 (2 : 1) gave a bi-phased aluminium borate–boron oxide (Al18B4O33·7B2O3) after calcination at >700 °C. The dried gels and oxide materials were all characterized by elemental analysis, TGA–DSC, and powder XRD.

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