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机构地区:[1]南京工业大学化学化工学院、材料化学工程国家重点实验室,南京210003
出 处:《无机化学学报》2009年第3期454-458,共5页Chinese Journal of Inorganic Chemistry
基 金:国家自然科学基金(No.20636020)资助项目
摘 要:在有机体系中电化学溶解钽得到有机前驱体钽醇盐,在30mL电解液中加入6mLH2O2和0.6g阳离子表面活性剂十六烷基三甲基溴化铵(CTAB),150℃溶剂热反应24h,产物经过高温热处理后得到Ta2O5空心微球。研究表明:溶剂热反应得到无定型Ta2O5纳米颗粒,600℃热处理后得到由纳米颗粒组装成的无定型Ta2O5半球结构,经过进一步的900℃高温热处理导致这些相邻半球结构进一步组装为斜方晶系的Ta2O5微米级空心球(直径约2μm),球壁厚度在150nm左右,空心部分直径约为1.5μm,球壁是由更小的Ta2O5纳米空心球组成;而在相同条件下,采用油酸代替CTAB,得到粒径减小的Ta2O5纳米颗粒。同时探讨了高温热诱导组装多孔Ta2O5微米空心球的可能形成机理。Amorphous Ta2O5 nanoparticles were solvothermally synthesized at 150℃ for 12 h in a mixed H2O2 and CTAB solution by using electrolyzed tantalum alkoxide as the starting material. The calcined samples were characterized by using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that amorphous Ta2O5 with hemispheres structure are obtained from nanoparticles after calcination at 600℃ for 5 h. Porous Ta2O5 microspheres are with an average diameter of 2 μm and a hollow cavity structure is self-assembled when subjecting to calcination at 900℃ for 5 h, the thickness of the hole is about 150 nm and the diameter of the hollow part is estimated to be 1.5 μm. However, the size of tantalum pentoxide is decreased after calcination at 600℃ and further decreased at 900 ℃ when anionic surfactant(oleic acid) is used instead of CTAB. The possible temperature-triggered microsphere assembly mechanism is discussed, and the abnormal phenomenon about the decreased tantalum pentoxide nano-particle is also reasonably interpreted.
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