Dong Wen-Sheng, Lin Feng-Qiang, Liu Chun-Ling, Li Meng-Yuan
Key Laboratory of Applied Surface and Colloid Chemistry (Shaanxi Normal University), Ministry of Education, and School of Chemistry and Materials Science, Shaanxi Normal University, Xi'an, 710062, China.
J Colloid Interface Sci. 2009 May 15;333(2):734-40. doi: 10.1016/j.jcis.2009.02.025. Epub 2009 Feb 13.
Zirconia precursor nanowires were synthesized via the solvothermal reaction of zirconium tetra-n-propoxide Zr(OPr(n))(4) with ethylene glycol and 1-butyl-3-methyl imidazolium tetrafluoroborate ionic liquid at 160 degrees C. The as-synthesized nanowires were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), thermogravimetric and differential scanning calorimetric (TG-DSC) analysis, and infrared spectroscopy (IR), etc. The length of the as-synthesized nanowires reaches approximately 20 mum, and the width approximately 50 nm, giving an aspect ratio of a few hundreds. Upon calcination at elevated temperatures, the zirconia precursor nanowires transform from relative dense structure into highly porous ZrO(2) nanowires consisting of interconnected nanocrystallites; in addition the length of the nanowires is greatly reduced. Cyclic voltammetry measurement shows that the modification of the graphite electrode with the ZrO(2) nanowires greatly enhances sensitivity of the detection of vanadium, suggesting that ZrO(2) nanowires may find important applications in vanadium(V) determination using electroanalytical methods with chemically modified electrode technique.
通过四正丙醇锆Zr(OPr(n))(4)与乙二醇以及1-丁基-3-甲基咪唑四氟硼酸盐离子液体在160℃下进行溶剂热反应合成了氧化锆前驱体纳米线。采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、粉末X射线衍射(XRD)、热重和差示扫描量热(TG-DSC)分析以及红外光谱(IR)等手段对合成的纳米线进行了表征。合成的纳米线长度约为20μm,宽度约为50nm,长径比为几百。在高温煅烧时,氧化锆前驱体纳米线从相对致密的结构转变为由相互连接的纳米微晶组成的高度多孔的ZrO(2)纳米线;此外,纳米线的长度大幅缩短。循环伏安法测量表明,用ZrO(2)纳米线修饰石墨电极极大地提高了钒检测的灵敏度,这表明ZrO(2)纳米线在采用化学修饰电极技术的电分析方法测定钒(V)方面可能具有重要应用。