本研究採用溶膠凝膠法，分別以二次乙基三胺(DETA)、二乙基胺(DEA)、二甲胺(DMA)、三甲基胺(TMA)為氮源，十六胺(HDA)為結構劑，異丙氧基鈦(TIP)為鈦的前驅物，使用聚焦式微波反應器，僅需190℃、一小時的溶熱反應，即可合成粒徑為400-600 nm、淡黃色的純銳鈦礦相N-TiO2介孔次微米球。從UV-Visible 吸收光譜圖發現，N-TiO2在可見光區域的光吸收率明顯較P25高。且經由XPS分析顯示，所得到的氮摻雜有兩種形式，分別為取代態和間隙態，表示氮有確實進入到TiO2晶格內，同時本研究也發現，氮鍵結的形式會隨著胺類螯合劑種類以及添加之Ti/N配比不同，而產生明顯的改變，同時也影響了次微米球的比表面積與光催化活性。最後，以羅丹明B水溶液在可見光(420nm)照耀下的脫色率作為光催化活性依據，發現N-TiO2的光催化活性比P25要高，且當氮以間隙型態（Ti-O-N）摻入的方式，較取代型態的方式（Ti-N）摻入，其在可見光的吸收愈高，而光催化效果也愈好。在本研究所合成之N-TiO2樣品中，以三甲基胺（TMA）作為氮源、且N/Ti添加莫耳比為0.9的樣品，因為其間隙型態的含氮量是所有N-TiO2樣品中最高的，因此具有最高的光催化效率。

In this study, a novel and facile method is developed to synthesize N-TiO2 mesoporous microspheres via microwave-assisted solvothermal reaction route. Sol-gel process using titanium isopropoxide as precursors, hexadecylamine as structure-directing agent, and diethylenetriamine、diethylamine、dimethylamine、trimethylamine as amine agents, respectively. The size of the microsphere was ranging from 400 to 600 nm in anatase phase can be obtained using the current method under 190℃ in 1 hour. A shift of the absorption edge to a lower energy and a stronger absorption in the visible light region were observed. Both substitutional and interstitial nitrogen-doped titanium dioxides were prepared. Their surface states were clarified by XPS spectra. The nitrogen bonding form changed from different N/Ti ratio and different amine agents, and the specific surface area、photodegradation was different. The results of photodegradation or the organic pollutant rhodamine B in the visible light irradiation (420 nm) suggested that the TiO2 photocatalysts after nitrogen doping were greatly improved compared with Degussa P-25. The results showed that the photodegradatio, and the trimethylamine (N/Ti ratio =0.9)was obviously prior to others N-doped TiO2, because its interstitial is the height in N-doped TiO2 sample. Moreover, the visible light activity of interstitial N-doped TiO2 is higher than that of
substitutional N-doped TiO2 .

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