采用溶胶-凝胶法,以正硅酸乙酯(TEOS)为硅源,通过TEOS的水解和缩合制备核壳结构γ-Fe2O3/SiO2的纳米复合材料。利用正交试验与单因素实验,研究了γ-Fe2O3、TEOS、氨水的用量、醇水比、反应时间、反应温度和搅拌速率对纳米复合材料合成的影响,并且对合成产品进行TEM、XRD、DSC、FTIR、粒径分析仪等表征分析。结果发现,对纳米复合材料合成效果影响最大的因素是TEOS的用量,最佳工艺方案为γ-Fe2O3用量为0.06 g、TEOS 0.5 mL、氨水2 mL、醇水体积比为5:1、反应时间为8 h、反应温度为30 ℃、搅拌速率为150 r/min; 以最佳合成方案合成的核壳结构γ-Fe2O3/SiO2与γ-Fe2O3相比,平均粒径减少34.1%,颗粒尺寸分布较为均匀,具有较好的分散性。
Abstract
Core-shell structural γ-Fe2O3/SiO2 nano composite particles were prepared via hydrolysis and condensation by sol-gel method using TEOS as silica precursor. Orthogonal design and single factor experiment were utilized to study effect of seven factors on the synthesis of nano composite particles, such as the dosage of γ-Fe2O3, Ammonia water, TEOS, the ratio of alcohol to water, reaction time, reaction temperature and stirring speed. The synthesized products were characterized by transmission electron microscope(TEM), X-ray diffraction(XRD), infrared spectrometer(FTIR), differential scanning calorimetry(DSC)and particle size analyzer. The results showed that the dosage of TEOS had the most influence on the synthesis of core-shell structural γ-Fe2O3/SiO2 nanocomposite particles. The optimum conditions were as follows:γ-Fe2O3 0.06 g, TEOS 0.5 mL, ammonia 2 mL, the ratio of alcohol to water 5:1, reaction time 8 h, reaction temperature 30 ℃ and stirring speed 150 r/min. Compared core-shell structural γ-Fe2O3/SiO2 with γ-Fe2O3, the average particle size was reduced by 34.1% and particle size distribution was more uniform, with good dispersion.
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基金
收稿日期:2012-09-18 修回日期:2013-04-11
基金项目:江苏省2011年度普通高校研究生科研创新计划项目(CXLX11_0530)
第一作者:陈磊,硕士生。*通信作者:景宜,教授。E-mail: jingyi@njfu.com.cn。
引文格式:陈磊,景宜. 核壳结构γ-Fe2O3/SiO2纳米复合材料的合成与分析[J]. 南京林业大学学报:自然科学版,2013,37(4):115-120.
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