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均匀沉淀法制备核-壳型TiO2@SbxSn1-xO2及其导电性能
引用本文:王亚男,钱建华,邢锦娟,陈宇昕. 均匀沉淀法制备核-壳型TiO2@SbxSn1-xO2及其导电性能[J]. 复合材料学报, 2019, 36(12): 2920-2931. DOI: 10.13801/j.cnki.fhclxb.20190327.001
作者姓名:王亚男  钱建华  邢锦娟  陈宇昕
作者单位:1.渤海大学 功能化合物的合成及应用辽宁省重点实验室, 锦州 121000;
基金项目:国家自然科学基金(21878024);辽宁省教育厅创新团队资助项目(LT2015001)
摘    要:以尿素为沉淀剂,采用均匀沉淀法包覆改性TiO2,制备了核壳型TiO2@SbxSn1-xO2(ATO)复合导电粉体,利用SEM、EDS、HRTEM、XRD、XPS、顺磁波谱仪(EPR)、FTIR及激光粒度仪(LPSA)等对其进行表征,并对其导电性的主要影响条件进行了研究及分析,提出了均匀沉淀包覆及反应机制。研究表明,反应温度为92℃时,尿素与金属阳离子摩尔比为10∶1的情况下,OH-释放量及释放速率适中,引入SO42-作为催化剂,降低金属阳离子成核能垒,且SO42-与Cl-最佳摩尔比为1∶25时,所得产品的纳米SbxSn1-xO2(ATO)壳层在TiO2表面包覆均匀连续完整,其厚度约为15 nm。当包覆完全时,随着Sb掺杂量增加,复合粉体电阻率降低,Sn与Sb摩尔比达到12∶1时,再增加Sb含量,其电阻率不变。最优制备条件下,复合粉体电阻率值为7.5 Ωcm,导电性能良好。 

关 键 词:均匀沉淀   TiO2   掺锑二氧化锡   包覆机制   电阻率
收稿时间:2018-12-20

Preparation and electrical conductivity of TiO2@SbxSn1-xO2 core-shell composite particles by homogeneous precipitation
Affiliation:1.Liaoning Province Key Laboratory of Synthesis and Application of Functional Compounds, Bohai University, Jinzhou 121000, China;2.Chemical Engineering and Environmental Engineering, Liaoning Shihua University, Fushun 113001, China
Abstract:Core shell conductive composite powders of TiO2 coated with SbxSn1-xO2 antimony-doped tin oxide(ATO) nanoparticles were prepared with urea as the precipitant by homogeneous precipitation. The as-prepared composite powders were characterized by SEM, EDS, HRTEM, XRD, XPS, electron paramagnetic resonance(EPR), FTIR and laser particle size analyzer(LPSA), respectively. Effects of several main experimental parameters on the resistivity of the TiO2@ATO powders were primarily investigated. A possible mechanism for coating of ATO nanoparticles on the surface of TiO2 microspheres was proposed. The results show that when the molar ratio of metal cation to urea for precipitation reaction is 1:10 at the temperature of 92℃, the release amount and rate of OH- are moderate. At the same time, SO42- was introduced as a catalyst to reduce the nucleation barrier of metal cations, in which the optimum molar ratio of SO42- to Cl- is 1:25. Uniform, continuous and compact shell layer of ATO of the obtained product is formed on the surface of the TiO2 with a thickness of approximately 15 nm. When completely covered, the resistivity of composite powders decreases first and then, when the molar ratio of Sn to Sb reaches 12:1, changes little with the increase of Sb doping amount. Under the optimum experimental conditions, TiO2@ATO has good electrical conductivity with the resistivity of 7.5 Ωcm. 
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