The Calcination Effect on the Crystallinity, Nitrogen Content, and Pore Structure of Nitrogen-Doped Titanium Dioxide

C. Kusumawardani
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Abstract

Mesoporous nitrogen-doped titanium dioxide nanomaterials have been synthesized through a one-step sol gel process with dodecylamine as the pore template as well as the nitrogen source. The calcination process plays an important role in the crystallization process, determination of doped nitrogen, and pore formation. The effect of calcination temperature on the material structure was studied by calcination treatment of the as-synthesized material at several temperature variations. The resulting materials were characterized using FTIR, XRD, XPS, and N2 gassorption analysis.  The results showed that the anatase TiO2 crystal structure began to form with calcination at 400 °C. The higher calcination temperature tends to cause the transformation of anatase crystal phase into rutile. The higher calcination temperature also affects the doped nitrogen content, where the pore-templating molecules begin to disappear at a calcination temperature and leaving a number of dopants on TiO2. All dopants are released from TiO2 at a calcination temperature of 600 °C. The optimum calcination temperature to form mesoporous structure was 450 °C, and the sintering occurs at a calcination temperature higher than optimum temperature indicated by the collapse of the pore structure.
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煅烧对氮掺杂二氧化钛结晶度、含氮量和孔隙结构的影响
以十二烷基胺为孔模板,以氮源为原料,通过一步溶胶凝胶法制备了介孔氮掺杂二氧化钛纳米材料。煅烧过程在结晶过程、掺杂氮的测定和孔隙形成中起着重要的作用。通过对合成材料在不同温度下的煅烧处理,研究了煅烧温度对材料结构的影响。用FTIR、XRD、XPS和N2吸附分析对所得材料进行了表征。结果表明:在400℃煅烧时,TiO2的锐钛矿型晶体结构开始形成;较高的煅烧温度有利于锐钛矿晶相向金红石晶相转变。较高的煅烧温度也影响了掺杂氮的含量,在煅烧温度下,孔模板分子开始消失,在TiO2上留下了大量的掺杂物。在600℃的煅烧温度下,所有的掺杂物都从TiO2中释放出来。形成介孔结构的最佳煅烧温度为450℃,烧结温度高于最佳温度,孔隙结构坍塌。
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