不同形貌MFe_2O_4（M=Mn，Zn，Co，Ni等）的合成及性能研究
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摘要
尖晶石铁氧体MFe2O4(M=Mn, Zn, Co, Ni, Cu)由于具有优良的物理化学性质和巨大的应用潜力而备受关注。研究发现铁氧体的形貌和尺寸会直接影响其结构和性质,但是铁氧体是一种结构复杂的三元氧化物,一般都需要在模板或表面活性剂辅助下经繁杂的操作过程才能合成出特殊形貌的产物。本论文在无需任何表面活性剂或模板的条件下合成出纳米棒状、纳米纤维状和橄榄球形尖晶石铁氧体,并用溶胶-凝胶法合成出三维大孔的尖晶石铁氧体。研究了不同形貌铁氧体的合成条件、结构、磁性和吸附性质,并探讨了一维铁氧体纳米纤维和三维大孔铁氧体的形成过程。而且将大孔铁氧体作为吸附剂应用在废水处理中,分析其吸附过程中的影响因素、吸附动力学及吸附平衡等温线等,探讨了铁氧体作为吸附剂处理有机染料废水和重金属离子废水的吸附机理。
本论文将种子生长法(以一定形貌的简单氧化物为原料,合成特殊形貌的复杂氧化物)与传统的水热法或固相法相结合,实现了从具有特殊形貌的二元氧化物合成特殊形貌的三元氧化物。在此合成过程中,先以简单的沉淀法方法合成出具有特殊形貌的二元氧化物,再将其作为种子用传统的水热法或固相法合成出纳米棒状、纳米纤维状和橄榄球形的尖晶石铁氧体。以此方法合成出的纳米棒状、纳米纤维状和橄榄球形铁氧体的形貌可以通过控制合成条件实改变,而且所得产物的磁性明显高于直接用市售氧化物为原料所得产物的磁性。另外,本论文探讨了种子在用此方法制备铁氧体过程中的作用,以及用固相-种子法合成纳米纤维状NiFe2O4时纳米纤维的形成过程。
以鸡蛋蛋清为络合剂用溶胶-凝胶法合成出三维大孔铁氧体MnFe2O4、NiFe2O4、ZnFe2O4、CoFe2O4。发现大孔铁氧体的合成条件对孔径大小和孔的形状有很大影响。探讨了以此方法合成大孔铁氧体时形成大孔的机理。
将大孔铁氧体作为吸附剂应用在有机染料和重金属离子废水处理中,结果表明大孔铁氧体对有机染料(亚甲基兰(MB)和碱性品红(FR))及重金属离子(Cu(II)、Cr(VI)和Ni(Ⅱ))都具有明显的吸附作用。由于所得尖晶石铁氧体具有明显的亚铁磁性,可以在外加磁场作用下容易地实现磁分离,铁氧体经分离和脱附后可以实现再生,并在多次吸附-脱附循环中保持较高的去除率。对铁氧体吸附有机染料的单因素影响吸附性能的实验进行了探讨,得出各种尖晶石铁氧体吸附MB和FR的最佳吸附条件。并通过吸附前后红外光谱分析、吸附动力学分析及吸附等温线分析,探讨了铁氧体吸附有机染料的吸附机理。结果表明铁氧体吸附MB和FR均符合准二级吸附动力学方程；均为颗粒内扩散和膜扩散联合控制过程；且均符合Langmuir吸附等温式。
研究了Zn2+离子掺杂对铁氧体MnFe2O4结构、形貌、磁性及吸附性质的影响,结果表明离子掺杂可以改变铁氧体的结构和形貌,适当掺杂有利于提高产物的磁性和吸附性质。
Spinel ferrites MFe2O4 (M=Mn, Zn, Ni et al.) have attached many attentions for their excellent physical and chemical properties. The nanoscale ferrites are applied widely in various fields with the development of nanotechnology. Since the structure and properties of ferrites can be affected by their morphologies, ferrites with different morphologies (nanorod, nanofibcr, olivary and pores) are synthesized by the routes of combining the suit growth method and simple hydrothermal/solid-state routes, without any template or active surfactant. The synthesis conditions, structures, morphologies, magnetic and adsorption properties are investigated. The formation mechanisms of NiFe2O4 nanofibers and 3D macroporous NiFe2O4 are studied. In addition, since the porous structure suit for adsorption, the porous ferrites are applied in the treatment of wastewater and the adsorption mechanism is studied by effect factors, adsorption kinetic and adsorption isothermal.
The syntheses of complex oxides using binary oxide as raw materials by simple routes are realized by combining the seed growth method and traditional hydrothermal/solid-state method. The special shape ferrites are difficult to synthesize without template or active surfactant due to their complex structures. However, the nanorod, nanofiber and olivary spinel ferrites are synthesized by seed-hydrothermal and seed-solid-state routes in this work. And the morphologies can be controlled by synthesis conditions. During this synthesis process, simple oxide are synthesized by coprecipitation firstly, and then used as seed to fabricate the ferrites with nanofiber and olivary morphologies. In addition, the mechanism of synthesizing nanofiber ferrite by seed-solid-state route is studied.
3D-macroporous ferrites are synthesized by sol-gel method with egg white as ligand. This realized the synthesis of 3D macroporous ferrites with simple route and by biologic raw materials. And find that the synthesis condition related to the pore size of porous ferrites. In addition, the mechanism of forming pores in the process of synthesizing spinel ferries by this route is pointed out.
The porous ferrites are applied in the treatment of wastewater containing organic dyes and heavy metal ions. The results showed that all ferrites have obvious adsorption of organic dyes (MB and FR) and heavy metal ions (Cu (Ⅱ), Cr (VI) and Ni (Ⅱ)). The ferrites can be separated from solution after adsorption easily, due to their ferromagnetic properties. The separated ferrites can be reused many times keeping high adsorption activities, and the rates of adsorption in the reused cycles are even higher than that in the first cycle. The best adsorption conditions are investigated by the studies of the effect factors of organic dyes adsorption on ferrites.In addition, the adsorption mechanism of organic dyes on ferrites is studied by FT-IR analysis, adsorption kinetic and adsorption isothermal. Results showed that the Fe-O bond of ferrite is responsible for good adsorption, the adsorptions of MB and FR fit pseudo-second-order kinetic model, Langmuir isotherm equation well.
The effects of ions substitution on ferrites'structure, morphologies, magnetic and adsorption properties are studied. Results showed that the ions substitution can change ferrites'structure and morphologies, and reasonable substitution can enhance their magnetic and adsorption properties.
本论文将种子生长法(以一定形貌的简单氧化物为原料,合成特殊形貌的复杂氧化物)与传统的水热法或固相法相结合,实现了从具有特殊形貌的二元氧化物合成特殊形貌的三元氧化物。在此合成过程中,先以简单的沉淀法方法合成出具有特殊形貌的二元氧化物,再将其作为种子用传统的水热法或固相法合成出纳米棒状、纳米纤维状和橄榄球形的尖晶石铁氧体。以此方法合成出的纳米棒状、纳米纤维状和橄榄球形铁氧体的形貌可以通过控制合成条件实改变,而且所得产物的磁性明显高于直接用市售氧化物为原料所得产物的磁性。另外,本论文探讨了种子在用此方法制备铁氧体过程中的作用,以及用固相-种子法合成纳米纤维状NiFe2O4时纳米纤维的形成过程。
以鸡蛋蛋清为络合剂用溶胶-凝胶法合成出三维大孔铁氧体MnFe2O4、NiFe2O4、ZnFe2O4、CoFe2O4。发现大孔铁氧体的合成条件对孔径大小和孔的形状有很大影响。探讨了以此方法合成大孔铁氧体时形成大孔的机理。
将大孔铁氧体作为吸附剂应用在有机染料和重金属离子废水处理中,结果表明大孔铁氧体对有机染料(亚甲基兰(MB)和碱性品红(FR))及重金属离子(Cu(II)、Cr(VI)和Ni(Ⅱ))都具有明显的吸附作用。由于所得尖晶石铁氧体具有明显的亚铁磁性,可以在外加磁场作用下容易地实现磁分离,铁氧体经分离和脱附后可以实现再生,并在多次吸附-脱附循环中保持较高的去除率。对铁氧体吸附有机染料的单因素影响吸附性能的实验进行了探讨,得出各种尖晶石铁氧体吸附MB和FR的最佳吸附条件。并通过吸附前后红外光谱分析、吸附动力学分析及吸附等温线分析,探讨了铁氧体吸附有机染料的吸附机理。结果表明铁氧体吸附MB和FR均符合准二级吸附动力学方程；均为颗粒内扩散和膜扩散联合控制过程；且均符合Langmuir吸附等温式。
研究了Zn2+离子掺杂对铁氧体MnFe2O4结构、形貌、磁性及吸附性质的影响,结果表明离子掺杂可以改变铁氧体的结构和形貌,适当掺杂有利于提高产物的磁性和吸附性质。
Spinel ferrites MFe2O4 (M=Mn, Zn, Ni et al.) have attached many attentions for their excellent physical and chemical properties. The nanoscale ferrites are applied widely in various fields with the development of nanotechnology. Since the structure and properties of ferrites can be affected by their morphologies, ferrites with different morphologies (nanorod, nanofibcr, olivary and pores) are synthesized by the routes of combining the suit growth method and simple hydrothermal/solid-state routes, without any template or active surfactant. The synthesis conditions, structures, morphologies, magnetic and adsorption properties are investigated. The formation mechanisms of NiFe2O4 nanofibers and 3D macroporous NiFe2O4 are studied. In addition, since the porous structure suit for adsorption, the porous ferrites are applied in the treatment of wastewater and the adsorption mechanism is studied by effect factors, adsorption kinetic and adsorption isothermal.
The syntheses of complex oxides using binary oxide as raw materials by simple routes are realized by combining the seed growth method and traditional hydrothermal/solid-state method. The special shape ferrites are difficult to synthesize without template or active surfactant due to their complex structures. However, the nanorod, nanofiber and olivary spinel ferrites are synthesized by seed-hydrothermal and seed-solid-state routes in this work. And the morphologies can be controlled by synthesis conditions. During this synthesis process, simple oxide are synthesized by coprecipitation firstly, and then used as seed to fabricate the ferrites with nanofiber and olivary morphologies. In addition, the mechanism of synthesizing nanofiber ferrite by seed-solid-state route is studied.
3D-macroporous ferrites are synthesized by sol-gel method with egg white as ligand. This realized the synthesis of 3D macroporous ferrites with simple route and by biologic raw materials. And find that the synthesis condition related to the pore size of porous ferrites. In addition, the mechanism of forming pores in the process of synthesizing spinel ferries by this route is pointed out.
The porous ferrites are applied in the treatment of wastewater containing organic dyes and heavy metal ions. The results showed that all ferrites have obvious adsorption of organic dyes (MB and FR) and heavy metal ions (Cu (Ⅱ), Cr (VI) and Ni (Ⅱ)). The ferrites can be separated from solution after adsorption easily, due to their ferromagnetic properties. The separated ferrites can be reused many times keeping high adsorption activities, and the rates of adsorption in the reused cycles are even higher than that in the first cycle. The best adsorption conditions are investigated by the studies of the effect factors of organic dyes adsorption on ferrites.In addition, the adsorption mechanism of organic dyes on ferrites is studied by FT-IR analysis, adsorption kinetic and adsorption isothermal. Results showed that the Fe-O bond of ferrite is responsible for good adsorption, the adsorptions of MB and FR fit pseudo-second-order kinetic model, Langmuir isotherm equation well.
The effects of ions substitution on ferrites'structure, morphologies, magnetic and adsorption properties are studied. Results showed that the ions substitution can change ferrites'structure and morphologies, and reasonable substitution can enhance their magnetic and adsorption properties.
引文
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