毛细撞击流反应器制备掺锑氧化锡纳米颗粒及其分散体的研究

发布时间：2018-04-08 19:28

  本文选题：毛细撞击流反应器　切入点：掺锑氧化锡(ATO)　出处：《北京化工大学》2015年硕士论文

【摘要】：二氧化锡作为一种典型的n型半导体材料,具有导电、抗腐蚀、热稳定性高等诸多优良特性,锑的掺杂能够大幅度降低其电阻率,并提高其透光率,因而掺锑氧化锡纳米颗粒及其分散体被广泛地应用于半导体材料、电池、导电薄膜、透明隔热玻璃、发光材料等诸多领域。毛细撞击流反应器作为一种新式的化工过程强化设备,具有高效的传质、传热和混合特性,在纳米材料的制备方面拥有广阔的应用前景。本文以SnCl4·5H2O和SbCl3作为原材料,采用共沉淀法,首先探究了毛细撞击流反应器制备ATO纳米颗粒的可行性。结果表明,毛细撞击流反应器能够在较短的时间内制备粒径较小、分布均一、形貌规则,且结晶度较高的ATO纳米颗粒。在可行性的基础上,运用毛细撞击流反应器制备ATO纳米颗粒前驱体,然后通过煅烧法制备ATO纳米颗粒。实验考察了掺杂度(Sb/Sn)、终点pH、体积流率和陈化方式等因素对ATO纳米颗粒制备结果的影响。在前驱体制备基础上引入水热法替代煅烧制备得到ATO纳米分散体,并探究了水热时间、水热温度、水热介质以及水热前洗涤操作对于分散体电性能和稳定性的影响。本实验通过单一变量法得到了颗粒制备过程的优化条件：Sb/Sn为1/10,终点pH范围为2-3,体积流率范围为90-120 mL·min-1,同时,超声陈化可极大缩短反应时间。在该条件下制备得到的ATO纳米颗粒粒径较小,在10 nm左右,形貌规则、均一,结晶度较高,且电性能优异,电阻率一般在100 Ω·cm以内；水热法制备ATO纳米分散体的优化条件：水热前应抽滤洗涤6次以上,水热介质以去离子水较佳,水热温度应高于180℃,水热时间不应低于16 h。在该条件下制备的ATO纳米分散体具有良好的稳定性,可静置较长时间,且对应颗粒电阻率较低,一般在200 Ω·cm左右。
[Abstract]:As a typical n-type semiconductor material, tin dioxide has many excellent properties, such as conductive, corrosion resistance, high thermal stability and so on. The doping of antimony can greatly reduce its resistivity and improve its transmittance.Therefore, antimony doped tin oxide nanoparticles and their dispersions are widely used in semiconductor materials, batteries, conductive films, transparent insulating glass, luminescent materials and so on.As a new type of chemical process strengthening equipment, capillary impinging flow reactor has high efficiency in mass transfer, heat transfer and mixing, and has a broad application prospect in the preparation of nanomaterials.In this paper, SnCl4 5H2O and SbCl3 were used as raw materials and coprecipitation method was used to investigate the feasibility of preparing ATO nanoparticles in capillary impingement flow reactor.The results show that the capillary impinging flow reactor can prepare ATO nanoparticles with small particle size, uniform distribution, regular morphology and high crystallinity in a short time.On the basis of feasibility, the precursor of ATO nanoparticles was prepared by capillary impinging flow reactor, and then ATO nanoparticles were prepared by calcination method.The effects of doping degree, pH, volume flow rate and aging mode on the preparation of ATO nanoparticles were investigated.Based on the preparation of precursor, hydrothermal method was introduced to prepare ATO nanocrystalline dispersion instead of calcination. The effects of hydrothermal time, hydrothermal temperature, hydrothermal medium and washing operation before hydrothermal treatment on the electrical properties and stability of the dispersion were investigated.In this experiment, the optimized conditions of particle preparation were obtained by single variable method: the ratio of SB / Sn was 1 / 10, the final pH was 2-3, and the volume flow rate was 90-120 mL min-1. At the same time, ultrasonic aging could greatly shorten the reaction time.The ATO nanoparticles prepared under these conditions are smaller in size, about 10 nm, regular in morphology, uniform in morphology, high in crystallinity, excellent in electrical properties, and the resistivity is generally within 100 惟 cm.The optimum conditions for the preparation of ATO nano-dispersion by hydrothermal method are as follows: before hydrothermal treatment, more than 6 times of filtration and washing should be carried out, the best hydrothermal medium should be deionized water, the hydrothermal temperature should be higher than 180 鈩，

本文编号：1723048