The photocatalytic activities of triple-layered Aurivillius phases, Bi 2A′NaNb3O12 (A ′=Sr, Ca) and Bi2CaNaTa3O12, and of protonated forms prepared from these Aurivillius phases through selective leaching of bismuth oxide sheets were investigated. UV-Vis diffuse reflectance spectra showed blue shifts of the adsorption edges upon selective leaching. Although none of the triple-layered Aurivillius phases were active for photocatalytic H2 evolution from a 20 vol% ethanol solution, all the corresponding protonated forms showed photocatalytic activities for H 2 evolution. The effects of the changes in electronic structures and interlayer surface creation on photocatalytic activities are discussed.
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