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溶剂热法低温合成EuS中空微球的研究

Investigation of Solvothermal Synthesis EuS Hollow Micorospheres at Low-temperature

【作者】 李鹏

【导师】 冯威; 罗昔贤;

【作者基本信息】 大连海事大学 , 凝聚态物理, 2012, 硕士

【摘要】 随着社会的发展,人们渴望制备出集多种功能于一身的新型功能材料,EuS作为一类具有亚铁磁性半导体功能材料,由于Eu原子4f电子层的电子跃迁和自旋导致EuS存在显著的法拉第效应和克尔效应,从而使得EuS具有独一无二的光学和磁学特性,有望应用于药物靶向载体材料、磁存储等领域。目前EuS的合成方法主要有高温固相法、高温固气法、高温溶剂热法等,这些方法存在合成温度高、成本高的缺点。针对这一弊端,本文提出了采用溶剂热法低温合成EuS晶体的方案,实验表明采用乙腈溶剂热法可显著地降低EuS晶体合成温度,且采用该法首次合成了EuS中空微球。本论文的主要研究内容概括如下:1.分别在乙腈溶剂、去离子水中合成了配合物(Phen)Eu(Et2CNS2)3·nH2O,通过综合比较,确定在去离子水中合成配合物(Phen)Eu(Et2CNS2)3·nH2O更加科学。通过对配合物进行元素分析,首次对配合物的结晶水数量进行了定量分析;2.通过(Phen)Eu(Et2CNS2)3·nH2O做溶剂热前驱物,分别探索了采用氯仿、苯、甲苯、乙腈、四氢呋喃、乙二胺、三乙胺、无水乙醇做溶剂热反应溶剂,发现只有采用乙腈在220℃的低温可以合成EuS晶体,比目前广泛采用的高温溶剂热法制备EuS晶体的温度还低70~80℃,且发现采用乙腈溶剂热法首次合成了EuS中空微球;3.探究了乙腈溶剂热条件对产物EuS的影响,发现加热源、温度、压强,前驱物溶液浓度的改变,会显著地影响EuS晶体结晶质量;而加热源、温度、压强又会显著影响产物的形貌。

【Abstract】 With the development of society, people are longing for preparing a new type of functional material which integrates multiple functions. As a ferromagnetic semiconductor functional material, EuS possess unique optical and magnetic properties since EuS owens Faraday effect and the Kerr effect which come from the electron transition and spin of Eu atom 4f electron, and thus EuS is expected to be used as carrier material for targeting drug and magnetic storage material field. The current synthesis methods of EuS including high temperature solid reaction process, high temperature gas solid method and high temperature hydrothermal method, which all need high synthesis temperature, or high cost. In this paper, we proposes a solvothermal method of synthesizing EuS crystal at low temperature, and the results show that the solvent thermal method using acetonitrile as solvent can reduce the synthesis temperature of EuS crystal obviously. At the same time, it is the first time to synthesis EuS microspheres by solvothermal method.The main research contents of this thesis are summarized as follows:1.(Phen)Eu(Et2CNS2)3·nH2O was synthesized in acetonitrile and deionized water respectively. Identifying that the synthesis of (Phen)Eu(Et2CNS2)3·nH2O in deionized water is more scientific through comprehensive comparison. Also the quantitative analysis for the quantity of the crystallize water of the complexes was undertook based on the elements analysis of the complex.2. We used chloroform, benzene, toluene, acetonitrile, tetrahydrofuran, ethanediamine, triethylamine and anhydrous ethanol as solvent in the preparation of EuS hollow microsphere, while the complex (Phen)Eu(Et2CNS2)3·nH2O was used as precursor. Finally,we found out that the EuS crystal can only be prepared in the solvent of acetonitrile at low temperature 220℃. And the reaction temperature was 70-80℃, lower than the reaction temperature of high temperature hydrothermal method now widely used in the synthesis of EuS crystal. Meanwhile, the EuS hollow microsphere was prepared in the solvent of acetonitrile by solvothermal method for the first time.3. Here we explores the effect of different thermal conditions on EuS product, and finally we find out that the heating source, temperature, pressure and the concentration of the precursor in acetonitrile solution can influence the crystal quality of EuS significantly. However, the heating source, temperature and pressure has significant effects on the morphology of the product.

  • 【分类号】TB383.1
  • 【被引频次】1
  • 【下载频次】188
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