稀土硫（氧）化物的热解法制备及其性能研究

发布时间：2018-03-23 19:10

本文选题：倍半硫化物　切入点：热解　出处：《大连海事大学》2011年硕士论文

【摘要】：近年来,由于稀土倍半硫化物在传输材料,荧光、激光、光学磁性仪器等方面的潜在的应用价值,使其备受关注。传统的稀土倍半硫化物的合成方法通常采用高纯度的镧系元素,并且使用高纯度的硫粉或者是硫化氢、二硫化碳等对环境产生较大污染源的化合物作为硫源。与此同时,使用的制备方法为前驱体热解法则需要在高沸点的有机溶剂中进行,而产物中由于存在着有机物热解生成的残余碳(C)而使产物不纯,颜色较黑。因此,针对以上方法的缺陷与不足,本论文采用比较简单的固相直接热解的方法,在以硫蒸汽作为脱碳剂的环境中制备了稀土硫化物和硫氧化物。具体工作内容如下： 1.在反应体系中引入氧气(空气),通过热解Ln[S2CN(C4H8)]3-phen (Ln=Gd, Yb,Ho)得到了产物Gd2O2S:Yb,Ho。利用红外光谱(FTIR)和光致发光(PL)光谱等多种分析测试手段对所得产物进行表征。确定得到的产物为单色性良好的绿色上转换发光材料。 2.在氩气和硫气氛的保护环境下直接热解Gd[S2CN(C4H8)]3-phen前驱体得到产物Gd2S3；通过X-射线衍射(XRD)、扫描电镜(SEM)等分析测试手段对样品进行表征,发现得到的产物纯度较高,粒径大小均一,硫气氛的引入可以有效的除去产物中的碳杂质。在低温制备条件下,样品呈现出黑色,随着温度升高,样品的颜色逐渐变为黄色。 3.加入与前驱体Gd(Phen)(Ddtc)3相同摩尔的铜试剂,经充分混合研磨后共同热解,得到了第三种产物NaGdS2。利用同样的测试方法分析后发现：产物的形貌为微米级类球形且纯度高,这也是一种制备三元稀土硫化物(NaReS2)的新方法。
[Abstract]:In recent years, due to its potential applications in transport materials, fluorescence, laser, optical magnetic instruments, etc. Traditional methods for the synthesis of rare earth times semisulfide are usually high purity lanthanide, and high purity sulfur powder or hydrogen sulfide, Compounds such as carbon disulfide, which produce a large source of pollution to the environment, are used as sulfur sources. At the same time, the preparation method used is that the precursor pyrolysis method needs to be carried out in organic solvents with high boiling point. However, the product was impure and black because of the existence of residual carbon dioxide (C) formed by pyrolysis of organic compounds. Therefore, in view of the defects and shortcomings of the above methods, this paper uses a simple solid phase direct pyrolysis method to prepare rare earth sulfides and sulfur oxides in the environment of sulfur vapor as decarbonizer. The specific work is as follows:. 1. The product Gd _ 2O _ 2S: Yb Hoh was obtained by introducing oxygen (air) into the reaction system by pyrolysis of Ln [S _ 2CNC _ 4H _ (8)] 3-phen (Ln). The products were characterized by FTIR and photoluminescence spectra. The obtained products were characterized by FTIR and photoluminescence spectra. Monochromatic green upconversion luminescent material. 2. The product Gd2S3 was obtained by direct pyrolysis of Gd [S2CNC4H8] 3-phen precursor under the protection of argon and sulfur atmosphere. The samples were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The carbon impurity in the product can be effectively removed by the introduction of sulfur atmosphere. Under the condition of low temperature preparation, the sample appears black, and with the increase of temperature, the color of the sample becomes yellow gradually. 3. The third product, NaGdS2, was obtained by adding copper reagent with the same mole as the precursor Gd(Phen)(Ddtc)3, and after fully mixed grinding, the third product NaGdS2 was obtained. It was found that the morphology of the product was micrometer spherical and the purity of the product was high. This is also a new method for the preparation of ternary rare earth sulfides (NaReS 2).
【学位授予单位】：大连海事大学
【学位级别】：硕士
【学位授予年份】：2011
【分类号】：O611.4

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