酒石酸辅助均匀沉淀法制备TiO2/氧化锡锑

Fabrication of TiO2/Sb-doped tin oxide composite by tartaric acidassisted homogeneous precipitation method

以TiO2为基核,结晶四氯化锡和三氯化锑为主要原料,尿素为沉淀剂,酒石酸(TA)为辅助剂,PVP(聚乙烯吡咯烷酮)为分散剂,通过均匀沉淀法制备TiO2/ATO复合导电粉体,考察络合剂及沉淀剂对复合粉体导电性能的影响,并对其反应机理进行探讨。采用扫描电镜(SEM)、透射电镜(TEM)、X线衍射(XRD)、能谱仪(EDS)、光电子能谱(XPS)及傅里叶变换红外光谱(FTIR)等对复合材料的微观形貌、物相结构及材料成分进行表征。研究结果表明:粒径约为12.3 nm的氧化锡锑粒子包覆在近球状金红石型TiO2表面,形成核壳复合结构,且各组成元素在复合材料中均匀分布。在本反应体系中,酒石酸作为中间体配体供体,同时尿素协同调节体系pH。当TA与Sb物质的量比为1:1,尿素与Sn物质的量比为5:1时,所制复合粉体具有最佳导电性能,其电阻率为6.85Ω·cm。

TiO2/Sb-doped tin oxide(ATO)composite conductive materials were prepared by tartaric acid-assisted homogeneous precipitation method using TiO2 as core,tin chloride pentahydrate and antimony trichloride as main materials,urea as precipitant,tartaric acid(TA)as auxiliary agent,and PVP(polyvinylpyrrolidone)as dispersing agent.The effects of precipitant and complexing agent on the conductivity of composite powder were investigated,and the reaction mechanism were discussed.The microstructure,phase structure and material composition of the obtained composite were characterized by scanning electron microscope(SEM),transmission electron microscope(TEM),X-Ray diffraction(XRD),energy disperse spectroscopy(EDS),X-ray photoelectron spectroscopy(XPS)and Fourier transform infrared spectroscopy(FTIR),respectively.The results show that ATO particles with the size of about 12.3 nm are coated on the surface of near?spherical rutile TiO2,forming a core?shell composite structure,and all constituent elements are evenly distributed in the composite.In this reaction system,tartaric acid provides the intermediate with ligands,and urea regulates the pH of the system.When the molar ratio of TA to Sb reaches 1:1 and that of urea to Sn is 5:1,the as-prepared TiO2/ATO has the excellent conductivity and its resistivity is 6.85Ω·cm.