超重力液相沉淀法制备纳米铁酸钴

doi:10.16085/j.issn.1000-6613.2017-1343

摘要/Abstract

摘要： 针对磁力搅拌器制备纳米材料时存在粒径分布宽、分散不均匀的问题，采用撞击流-旋转填料床结合化学共沉淀法，以Fe（NO₃）₃·9H₂O、Co（NO₃）₂·6H₂O、NaOH为原料制备CoFe₂O₄纳米颗粒。研究了转速、液体流量、NaOH浓度以及晶化时间对CoFe₂O₄纳米颗粒粒径的影响；并与磁力搅拌器制备的CoFe₂O₄纳米颗粒在磁性能方面进行了对比。采用X射线衍射仪（XRD）、傅里叶红外光谱仪（FTIR）、透射电镜（TEM）、纳米粒度仪及振动样品磁强计（VSM）对产物的粒径形貌及磁性能进行表征。结果表明：CoFe₂O₄纳米颗粒的粒径随转速、液体流量和NaOH浓度的增加而减小，但随晶化时间的增加而增大。最佳工艺条件为：转速900r/min，液体流量60L/h，NaOH浓度3mol/L，晶化时间6h。此条件下制备的CoFe₂O₄纳米颗粒的粒径约为20nm，饱和磁化强度为75.43emu/g，较磁力搅拌器提高40%。

关键词: 超重力, 化学共沉淀, 撞击流-旋转填料床, 铁酸钴, 纳米粒子

Abstract: Nanoparticles prepared by magnetic stirrer tend to have a wide particle size distribution and uneven dispersion. In order to address these problems,CoFe₂O₄ nanoparticles were prepared by chemical coprecipitation in impinging stream-rotating packed bed (IS-RPB) using aqueous solutions of Fe (NO₃)₃/Co (NO₃)₂ and NaOH as raw materials. The effects of rotational speed,liquid flow rate,NaOH concentration and crystallization time on the particle size of CoFe₂O₄ nanoparticles were examined,and their magnetic properties were compared with that prepared by magnetic stirrer. The particle size,morphology and magnetic properties of as prepared nanoparticles were characterized by X-ray diffraction (XRD),fourier infrared spectroscopy (FTIR),transmission electron microscopy (TEM),nanoparticle size analyzer and vibrating sample magnetometer (VSM). The results showed that the particle size of CoFe₂O₄ nanoparticles decreases with the increase of rotational speed,liquid flow rate and NaOH concentration,but increases with the increase of crystallization time. The optimum operating conditions are as follows:rotational speed 900r/min,liquid flow rate 60L/h,NaOH concentration 3mol/L,and crystallization time 6h. CoFe₂O₄ nanoparticles prepared under optimum operating conditions have an irregular shape with an average diameter of about 20nm and a saturation magnetization of 75.43emu/g,which is 40% higher than that prepared by magnetic stirrer.

Key words: high gravity, chemical coprecipitation, impinging stream-rotating packed bed, cobalt ferrite(CoFe₂O₄), nanoparticles

中图分类号:

TQ586

祁贵生, 武晓利, 刘有智, 郑奇, 郭林雅. 超重力液相沉淀法制备纳米铁酸钴[J]. 化工进展, 2018, 37(05): 1680-1686.

QI Guisheng, WU Xiaoli, LIU Youzhi, ZHENG Qi, GUO Linya. Preparation of cobalt ferrite nanoparticles by high gravity liquid precipitation method[J]. Chemical Industry and Engineering Progress, 2018, 37(05): 1680-1686.

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