| 3-氨基丙醇调控合成超顺磁四氧化三铁微球 |
| Tunable Synthesis of Superparamagnetic Magnetite Microspheres by 3-Aminopropanol |
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| 摘要: 采用乙二醇为溶剂,无水FeCl3为铁源,聚丙烯酸为稳定剂,通过改变3-氨基丙醇的用量,合成了一系列不同微球直径和晶粒大小的超顺磁Fe3O4微球。高分辨率透射电镜和X-射线衍射分析证实所得产物为Fe3O4,红外光谱和热重分析表明,微球表面成功包覆聚丙烯酸。微球的大小和组成微球的颗粒粒径分别用透射电镜和X-射线衍射分析,结果表明,所得微球的直径随着3-氨基丙醇的用量增加而减小,组成微球的颗粒粒径随着3-氨基丙醇的用量增加而增大。磁性测试表明所制备微球室温下具有良好的超顺磁性。该制备方法步骤简单,可望用于其他无机氧化物纳米微球或颗粒的制备。 |
| 关键词: 3-氨基丙醇 可控制备 超顺磁性 四氧化三铁 微球 |
| 基金项目: 国家自然科学基金(No.51302151)、福建省卫生教育联合攻关计划(No.WKJ-FJ-36)、福建省科技厅重点项目(No.2012Y0061)资助项目。 |
| Abstract: We report a polyol process for the synthesis of superparamagnetic magnetite microspheres with tunable size of the primary nanograins and the secondary structural ones. In a typical synthesis, FeCl3 (1 mmol) and polyacrylic acid (PAA, 2 mmol) were dissolved in ethylene glycol (EG, 12 mL) and 3-aminopropanol (3 mL) was added subsequently. Then the mixed solution were sealed in a Teflon lined stainless-steel autoclave (20 mL capacity) and heated at 200 ℃ for 6 h. The diameter of the microspheres and the grain particle size can be tuned spontaneously by changing the ratio of EG to 3-aminopropanol. The microspheres diameter decreases from 370 nm to 150 nm while the grain particle size increases from 3 nm to 12 nm with the increase of the volume ratio of EG to 3-aminopropanol from 14:1 to 7.5:7.5. PAA and 3-aminopropanol acted as stabilizer and hydrolysis, respectively. PAA is remained unchanged in this process, so the size tuning is attributed to the changing of alkalinity with the ratio of EG to 3-aminopropanol. The crystal phase of magnetite microspheres were testified by high resolution transmission electronic microscope (HRTEM) and X-ray diffraction pattern (XRD). The diameter and its distribution of the microspheres was determined by TEM. The size of the grain particles was determined by XRD and infer from Scherrer formula. Fourier transform infrared spectroscopy (FT-IR) spectra exhibited the characteristic absorption peaks of carboxyl group, such as 1 634 cm-1 attributed to the Stretching vibration of-C=O, 1 548 cm-1 and 1 393 cm-1 due to the-COO-symmetric and antisymmetric stretching, respectively, suggesting PAA is bonded on the surface of the grain particles covalently through the interaction between the COO-group of PAA and the Fe atom. Thermal gravimetric analysis (TGA) indicates that two weight loss stages from 150 to 450 ℃ and 450~900 ℃ are due to the decomposition of the carbon chain and the carboxyl bonded on the surface of the particles, respectively. The magnetization curves of the microspheres were recorded by a vibration sample magnetometer (VSM). The coercivity force is almost negligible at 298 K, revealing that the microspheres is superparamagnetic at room temperature. This facile process can be also used for the synthesis of other inorganic oxide nanoparticles or microspheres. |
| Keywords: 3-aminopropanol tunable synthesis superparamagentic mageneite microspheres |
| 投稿时间：2014-05-26 修订日期：2014-07-25 |
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| 肖旺钏,王叶敏,王仁章,张丽华,郑可利.3-氨基丙醇调控合成超顺磁四氧化三铁微球[J].无机化学学报,2014,30(11):2559-2563. |
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