(111)-layered Ba5Ta4O_(15) photocatalysts were synthesised by a solid state reaction route and a citrate synthesis route, and their structural and electronic properties were investigated. After citrate route preparation, the presence of a second phase, namely Ba3Ta5O_(15), was determined by X-ray powder diffraction and absorption spectroscopy. The existence of this phase had a profound effect on the photocatalytic activity of this Ba5Ta4O_(15)/Ba3Ta5O_(15) composite in comparison to the pure Ba5Ta4O_(15) materials. The photocatalytic performance of the barium tantalates was evaluated by investigating the capability in 'OH radical formation and hydrogen generation. Strongly increased hydrogen evolution rates for the Ba5Ta4O_(15)/Ba3Ta5O_(15) composite, up to 160 higher than for the pure Ba5Ta4O_(15), were determined, and only very small amounts of Rh co-catalyst, deposited on the photocatalysts by stepwise reductive photo-deposition, were needed to achieve these results.
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