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五氧化二钒薄膜的溶胶凝胶法制备与性质研究
其他题名The preparation and character research of Vanadium pentoxide thin films by sol-gel
甄恩明
导师徐刚
2009-05-31
学位授予单位中国科学院广州能源研究所
学位授予地点广州能源研究所
学位名称硕士
关键词五氧化二钒薄膜 溶胶凝胶 二乙酰丙酮氧钒 C轴生长 非晶衬底
摘要氧钒化合物因其具有重要的特性而被人们广泛的研究。其中V2O5因为其良好的催化特性,而被广泛用作各种化学反应的催化剂。同时V2O5也具有很好的电化学性能,理论上,V2O5晶体中平均一个钒原子可以接受两个金属锂原子,具有良好的嵌锂性能,这使得把V2O5用作高容量锂离子电池的阴极膜有很大的吸引力。在电致变色方面作为离子储存膜,也得到了应用。 本课题采用sol-gel方法,以二乙酰丙酮氧钒和五氧化二钒粉末为前驱物,制备得到了钒的有机溶胶和无机溶胶,通过提拉和旋涂两种涂膜方式得到湿的凝胶膜,通过不同条件下的热处理,得到了五氧化二钒薄膜。利用傅立叶变换红外吸收光谱仪和热重分析仪研究了二乙酰丙酮氧钒溶胶的性质,探讨了溶胶的粘度、热处理温度、热处理气氛和陈化时间对薄膜的影响。通过X射线衍射分析,傅立叶变换红外光谱分析及UV-VIS-NIR光谱表征了五氧化二钒薄膜的结晶性和光学特性。 热分析表明二乙酰丙酮氧钒在氮气中300℃开始分解,在空气中250℃开始分解,据此,本实验的热处理温度选为350-550℃之间。二乙酰丙酮氧钒凝胶膜可以在空气,氮气中退火得到多晶五氧化二钒薄膜,在提纯的氮气以及氩氢气中得到的是非晶态的五氧化二钒薄膜。实验中得到的多晶五氧化二钒薄膜均沿着c轴生长。薄膜垂直于衬底平面生长,晶粒大小在24-45nm之间。所得薄膜的禁带宽度为2.0-2.4ev之间。随着热处理气氛中氧分压的减小,薄膜的附着力增大,空气中热处理获得的样品在受潮后容易脱落,而在提纯氮气中热处理得到的样品能耐受研磨;颜色由淡黄向暗绿色转变。
其他摘要Vanadium oxides have been studied because of its some important properties. Vanadium pentoxide has been used widely as its fine catalytic properties. Meanwhile, Vanadium pentoxide also has fine electrochemical property. Theoretically a Vanadium atom in Vanadium pentoxide crystal can accept two Li ions. Vanadium pentoxide is an attractive cathode material in high capacity Li ions rechargeable battery. Vanadium pentoxide can be also used as ions storage layer in Electrochromic devices. Vanadium pentoxide thin films were obtained in this subject by sol-gel method. The precursors in this project are Vanadium pentoxide powder and Vanadyl acetylacetonate. First, we prepare inorganic sol and organic sol by Vanadium pentoxide powder and Vanadyl acetylacetonate respectively. Then the gel thin films were prepared by dip-coating and spin-coating. Gel films were heat treated at definite conditions and Vanadium pentoxide thin films were synthesized. The properties of Vanadyl acetylacetonate sol was analyzed by FT-IR and DG-DSC. The Crystallinity and optical property of Vanadium pentoxide thin films were analyzed by X-ray diffraction, FT-IR spectrum and UV-VIS-NIR spectrum. The DG-DSC analysis reveals that Vanadyl acetylacetonate decomposes at 250oC and 300oC in nitrogen ambience and air respectively. In this subject, the heat treatment temperature was choosen between 350-550oC. Polycrystalline Vanadium pentoxide thin films were synthesized by heat treating Vanadyl acetylacetonate gel films in air and nitrogrn ambience. Amorphous Vanadium pentoxide thin films were synthesized by heat treating Vanadyl acetylacetonate gel films in argon and hydrogen misture ambience and purified nitrogen ambience. Polycrystalline Vanadium pentoxide thin films synthesized in this object have highly c-axis oriented nano V2O5 structures with grain diameter ranging from 21nm to 45nm. Polycrystalline Vanadium pentoxide thin films grow perpendicularly to the substrate. The optical band gap of Vanadium pentoxide thin films is between 2.0-2.4ev. The adhesion of Vanadium pentoxide thin films becomes stronger when the oxygen pressure increases in heat treatment atmosphere. The Vanadium pentoxide thin films obtained in air can shed after surface wetting. While the Vanadium pentoxide thin films obtained in nitrogen can bear grinding. The color of Vanadium pentoxide thin films varies from light yellow to light green as the oxygen pressure decrease in heat treatment atmosphere.
页数77
语种中文
文献类型学位论文
条目标识符http://ir.giec.ac.cn/handle/344007/5868
专题中国科学院广州能源研究所
推荐引用方式
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甄恩明. 五氧化二钒薄膜的溶胶凝胶法制备与性质研究[D]. 广州能源研究所. 中国科学院广州能源研究所,2009.
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