本文選題：倍半硫化物　切入點(diǎn)：熱解　出處：《大連海事大學(xué)》2011年碩士論文

【摘要】：近年來(lái),由于稀土倍半硫化物在傳輸材料,熒光、激光、光學(xué)磁性儀器等方面的潛在的應(yīng)用價(jià)值,使其備受關(guān)注。傳統(tǒng)的稀土倍半硫化物的合成方法通常采用高純度的鑭系元素,并且使用高純度的硫粉或者是硫化氫、二硫化碳等對(duì)環(huán)境產(chǎn)生較大污染源的化合物作為硫源。與此同時(shí),使用的制備方法為前驅(qū)體熱解法則需要在高沸點(diǎn)的有機(jī)溶劑中進(jìn)行,而產(chǎn)物中由于存在著有機(jī)物熱解生成的殘余碳(C)而使產(chǎn)物不純,顏色較黑。 因此,針對(duì)以上方法的缺陷與不足,本論文采用比較簡(jiǎn)單的固相直接熱解的方法,在以硫蒸汽作為脫碳劑的環(huán)境中制備了稀土硫化物和硫氧化物。具體工作內(nèi)容如下： 1.在反應(yīng)體系中引入氧氣(空氣),通過(guò)熱解Ln[S2CN(C4H8)]3-phen (Ln=Gd, Yb,Ho)得到了產(chǎn)物Gd2O2S:Yb,Ho。利用紅外光譜(FTIR)和光致發(fā)光(PL)光譜等多種分析測(cè)試手段對(duì)所得產(chǎn)物進(jìn)行表征。確定得到的產(chǎn)物為單色性良好的綠色上轉(zhuǎn)換發(fā)光材料。 2.在氬氣和硫氣氛的保護(hù)環(huán)境下直接熱解Gd[S2CN(C4H8)]3-phen前驅(qū)體得到產(chǎn)物Gd2S3；通過(guò)X-射線衍射(XRD)、掃描電鏡(SEM)等分析測(cè)試手段對(duì)樣品進(jìn)行表征,發(fā)現(xiàn)得到的產(chǎn)物純度較高,粒徑大小均一,硫氣氛的引入可以有效的除去產(chǎn)物中的碳雜質(zhì)。在低溫制備條件下,樣品呈現(xiàn)出黑色,隨著溫度升高,樣品的顏色逐漸變?yōu)辄S色。 3.加入與前驅(qū)體Gd(Phen)(Ddtc)3相同摩爾的銅試劑,經(jīng)充分混合研磨后共同熱解,得到了第三種產(chǎn)物NaGdS2。利用同樣的測(cè)試方法分析后發(fā)現(xiàn)：產(chǎn)物的形貌為微米級(jí)類球形且純度高,這也是一種制備三元稀土硫化物(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).
【學(xué)位授予單位】：大連海事大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2011
【分類號(hào)】：O611.4

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