锌铁氧体高温热解制备研究

发布时间：2018-12-10 10:34

【摘要】：锌掺杂的铁氧体(ZnxFe1-x)Fe2O4磁性纳米颗粒具有远比传统Fe3O4磁性纳米颗粒更强的磁性,更强的感应升温能力,和更高的磁共振弛豫率。因此,在生物医学应用,特别是肿瘤的造影和磁感应热疗等领域,锌铁氧体具有广泛的应用前景和巨大的应用潜力。在本文中,我们使用乙酰丙酮锌和乙酰丙酮铁作为前驱物,油酸作为表面活性剂,二苄醚作为溶剂,进行锌铁氧体磁性纳米颗粒的高温热解法制备。我们创新性地采用热注入法来进行锌铁氧体磁性纳米颗粒的高温热解制备,从而达到提升锌掺杂水平的效果。我们通过一系列系统的实验和表征,对高温热解法中不同反应条件对锌铁氧体磁性纳米颗粒的粒径、形貌、锌掺杂和包括磁感应升温能力,饱和磁化强度和MRI磁共振造影r2弛豫率在内的磁学性能的影响进行探究。我们先保持前驱物投料量不变,观察油酸投料量的改变对锌铁氧体的尺寸与形貌及锌掺杂水平和磁学性能的影响。结果表明,随着表面活性剂量的增加,锌铁氧体磁性纳米颗粒的尺寸、反应速度和锌掺杂水平呈现非单调的变化趋势。之后我们还进行了高性能锌铁氧体磁性纳米颗粒放量生产的探索,我们保持乙酰丙酮锌：乙酰丙酮铁：总油酸的比例不变,生长温度和升温速率不变,仅增加油酸和乙酰丙酮锌、乙酰丙酮铁的投入总量,对制得的锌铁氧体磁性纳米颗粒的尺寸、形貌、锌掺杂水平及磁学性能进行评估。结果表明,增加反应物的投入总量,可以有效实现放量制备锌掺杂铁氧体磁性纳米颗粒,并且获得优异的形貌及磁学性能。这对高性能锌铁氧体磁性纳米颗粒高温热解法放量生产具有指导意义。在最后一章中,我们合成了能在317K变色的Cu(dieten)2(ClO4)2配合物分子,接下来使用一块嵌有磁性纳米颗粒的结冷胶(Gellan gel)作为组织模型,来进行磁致热变色的研究,从而模拟该配合物分子在肿瘤热疗热剂量控制上的应用。实验结果表明,该配合物分子变色与复色反应灵敏,颜色变化明显,非常适合应用于作为肿瘤热疗热剂量控制的一个直观的定性的表征手段。
[Abstract]:The zinc-doped ferrite (ZnxFe1-x) Fe2O4 magnetic nanoparticles have much stronger magnetic properties than traditional Fe3O4 magnetic nanoparticles, stronger inductive heating capacity, and higher magnetic resonance relaxation rate. Therefore, zinc ferrite has a wide application prospect and great potential in biomedical applications, especially in tumor imaging and magnetic induction hyperthermia. In this paper, zinc acetylacetone and iron acetylacetone were used as precursors, oleic acid as surfactant and dibenzyl ether as solvent to prepare zinc ferrite magnetic nanoparticles by pyrolysis at high temperature. The thermal injection method was used to prepare the magnetic nanoparticles of zinc ferrite at high temperature so as to improve the doping level of zinc. Through a series of systematic experiments and characterization, the particle size, morphology, zinc doping and magnetic induction heating ability of zinc ferrite magnetic nanoparticles under different reaction conditions in pyrolysis at high temperature were investigated. The effects of saturation magnetization and MRI magnetic resonance imaging r 2 relaxation rate on magnetic properties were investigated. The influence of the amount of oleic acid on the size and morphology of zinc ferrite, zinc doping level and magnetic properties was observed. The results show that the size, reaction rate and zinc doping level of magnetic nanocrystals of zinc ferrite show a non-monotonic trend with the increase of surfactant content. Then we explored the production of high performance zinc ferrite magnetic nanoparticles. We kept the ratio of zinc acetylacetone to iron acetylacetone to total oleic acid constant, and the growth temperature and heating rate were constant. The size, morphology, zinc doping level and magnetic properties of the prepared zinc ferrite nanoparticles were evaluated by increasing the total input of oleic acid and acetylacetone zinc and iron acetylacetone. The results show that increasing the total amount of reactants can effectively realize the preparation of zinc-doped ferrite magnetic nanoparticles and obtain excellent morphology and magnetic properties. This is of guiding significance for the production of high temperature pyrolysis discharge of high performance zinc ferrite magnetic nanoparticles. In the last chapter, we synthesized Cu (dieten) _ 2 (ClO4) _ 2 complex molecules that can discolor at 317K, and then we used a chilled (Gellan gel) with magnetic nanoparticles as the structure model to study the magnetochromic discoloration. Thus, the application of the complex molecule in the hyperthermia dose control of tumor was simulated. The experimental results show that the complex is sensitive to color change and has obvious color change. It is suitable for use as an intuitive qualitative characterization method for the control of hyperthermia dose of tumor.
【学位授予单位】：东南大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TM277

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