Centre for Nanoscience and Technology, Department of Physics, Periyar University, Salem 636 011, Tamilnadu, India.
Talanta. 2011 Sep 30;85(4):2166-74. doi: 10.1016/j.talanta.2011.07.063. Epub 2011 Jul 23.
Nanocrystalline tungsten oxides (WO(3-δ)) are currently receiving a lot of attention because of their interesting electrical, magnetic, optical and mechanical properties. In this report, we present the synthesis of PEG assisted tungsten oxide (WO(3)) nanoparticles by simple household microwave irradiation (2.45 GHz) method. The samples were characterized using powder X-ray diffraction (XRD), thermal analysis (TG/DTA), transmission electron microscopy (TEM), UV-visible diffusion reflectance spectroscopy (UV-VIS-DRS), cyclic voltammetry and electrochemical impedance spectroscopy. Powder XRD results revealed that both the samples prepared with and without surfactant crystallize in the orthorhombic structure corresponding to WO(3) · H(2)O phase. Subsequent annealing under identical conditions (600°C/air/6h) led to significantly different products i.e. monoclinic W(17)O(47) from surfactant free sample and orthorhombic WO(3) from PEG assisted sample. Blue emission was observed through UV-VIS-DRS with blue shift and the band gap energy was estimated as 2.7 and 3.28 eV for PEG assisted as prepared (WO(3) · H(2)O) and annealed samples (WO(3)) respectively. Electrochemical measurements have been performed on all the samples deposited on the surface of glassy carbon (GC) electrode which showed high sensitivity and good selectivity for PEG assisted sample (WO(3) · H(2)O) for the direct detection of L-dopa.
纳米晶氧化钨(WO(3-δ))因其具有有趣的电学、磁学、光学和机械性能而受到广泛关注。在本报告中,我们提出了一种通过简单的家用微波辐射(2.45GHz)方法合成聚乙二醇辅助氧化钨(WO(3))纳米粒子的方法。采用粉末 X 射线衍射(XRD)、热分析(TG/DTA)、透射电子显微镜(TEM)、紫外可见漫反射光谱(UV-VIS-DRS)、循环伏安法和电化学阻抗谱对样品进行了表征。粉末 XRD 结果表明,未经表面活性剂处理和经表面活性剂处理的样品均以 WO(3)·H(2)O 相的正交结构结晶。在相同条件(600°C/空气/6h)下进一步退火导致明显不同的产物,即无表面活性剂的样品生成单斜相 W(17)O(47),而 PEG 辅助的样品生成正交相 WO(3)。通过 UV-VIS-DRS 观察到蓝移的蓝发射,PEG 辅助的未退火(WO(3)·H(2)O)和退火样品(WO(3))的带隙能量分别估计为 2.7 和 3.28eV。所有样品都沉积在玻璃碳(GC)电极表面上进行电化学测量,结果表明,对于直接检测 L-多巴,PEG 辅助的样品(WO(3)·H(2)O)具有高灵敏度和良好的选择性。