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Single phases of Inl-xNixTaO4 were synthesized by a solid-state reaction at 1,100 ℃, using pre-dried In2O3, Ta2O5 and NiO (99.99% purity) as starting materials. To increase the photocatalytic activity of the materials, we used impregnation with aqueous Ni(NO3)2 or RuC13 solution to load the oxide semiconductor surface with 1.0 wt% partly oxidized nickel or RuO2; these loaded materials act as electron traps and hydrogen evolution sites. The Ni-loaded photocatalysts were calcined at 350 ℃ for 1 h in air and reduced in H2 atmosphere (200 torr) at 500 ℃ for 2 h, then treated in O2 atmosphere (100 torr) at 200 ℃ for 1 h. The reduction-oxidation treatment produced a double-layered structure of metallic Ni and NiO (denoted NiOy) on the surface of the photocatalyst; this double-layered structure suppresses the backward reaction of water splitting, which is activated by metallic nickel surfaces. The Ru-loaded photocatalysts were calcined at 500 ℃ for 2 h in air. The water-splitting experiments were carried out with 0.5 g powdered photocatalyst suspended in 250 ml of pure water in a Pyrex glass cell. A 300-W Xe arc lamp was focused through a shutter window and a 420 nm long pass filter was placed on the surface of the cell. The gases evolved were determined by the thermal conductivity detector (TCD) gas chromatograph, which was connetted to the glass-made gas circulating line attached to the Pyrex glass cell. The results of the photocatalytic reaction and photophysical parameters are listed in Table 1. The non-doped catalyst, NiOy/InTaO4 is active, but the activity was significantly enhanced by Ni doping of InTaO4. As a typical example, Fig. 2 shows the evolution of H2 and O2 from pure water containing suspensions of NiOy/In0.9Ni0.1Ta0.4 and RuO2/In0.9Ni0.1TaO4 under visible light irradiation (λ>420 nm). The rates of H2 and O2 evolution were about 16.6 and 8.3 μmolh-1, respectively, and the quantum yield at 402 nm was estimated to be 0.66% by using an interference filter (λ=402 nm; half-width, 15.3 nm). For RuO2/In0.9Ni0.1TaO4, the rates of H2 and O2 evolution were about 8.7 and 4.3 μmolh-1,respectively. The gas formation rate of the NiOy loaded sample is about twice as large as that of the RuO2-loaded sample. The gas evolution stopped when the light was turned off, showing that the reaction is induced by the absorption of visible light and not by tribological processes, such as the so-called mechano-catalysis. |
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syy911: 金币+30, 翻译EPI+1, ★★★★★最佳答案, 非常感谢！ 2013-01-28 17:51:35
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使用预先干燥的In2O3， Ta2O5和氧化镍（99.99%纯度）作为原始材料，通过1100℃的固态反应将Inl-xNixTaO4的各个单极进行合成。为提升材料的光催化活动，我们使用含水的Ni(NO3)2 或者RuC13溶液进行注入，将氧化物半导体表层注入1%重量的部分氧化的镍或者RuO2；这些被载入的材料成为电子陷阱，是产生氢的场所。将注入了镍的光催化剂以350℃的温度在空气中焙烧1小时，然后在氚气（200托）中以500℃的温度还原2小时，再将其在氧气（100托）中以200℃的温度处理1小时。这种氧化还原处理在光催化剂表面产生一个双层的金属镍和氧化镍（NiOy）结构；这种双层结构抑制了由氧化镍表层激活的水裂解的逆向反应。将注入了钌的光催化剂在空气中以500℃的温度焙烧2小时。 进行水裂解实验，将0.5g粉末光催化剂放入盛有250ml纯净水的派热克斯玻璃比色槽中。使用一个300瓦的Xe弧光灯透过挡板窗照射，并将一个420mm的长通滤波器放在玻璃比色槽表面。所生成的气体由热导检测器的气相色谱仪决定，此热导检测器的气相色谱仪与一个玻璃的气体循环线相连，而该气体循环线附着于派热克斯玻璃比色槽。 关催化反应的结果和溶剂参数列在表一中。没有掺杂过的催化剂，NiOy/InTaO4 很活跃，但是该活动显著的被InTaO4中注入的镍加强了。一个很典型的例子，图表2表示在可见光照射下（λ>420 nm），含有NiOy/In0.9Ni0.1Ta0.4 和 RuO2/In0.9Ni0.1TaO4悬浮液的纯净水生成的氚和氧。氚和氧的生成率分别为16.6 μmolh-1和8.3 μmolh-1，在402 nm的情况下使用干涉滤光片时，量子产率预计可达到0.66%。 (λ=402 nm; 半宽度, 15.3 nm)。而对于RuO2/In0.9Ni0.1TaO4，氚和氧的生成率分别是约8.7 μmolh-1和8.7 and 4.3 μmolh-1。被注入NiOy的样本的气体生成速率是载有RuO2样本的两倍。当光被切断时，气体的生成便停止，这说明此反应由对可见光的吸收诱导，而非所谓的机械催化或摩擦过程。 |
2楼2013-01-28 14:42:26