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辐照作用下 1-乙基-3-甲基咪唑双(三氟甲基磺酰基)亚胺室温离子液体近表面化学成分的变化。

Changes of the near-surface chemical composition of the 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide room temperature ionic liquid under the influence of irradiation.

机构信息

Institute of Physics and Institute of Micro- and Nanotechnologies, TU Ilmenau, P.O. Box 100 565, 98684 Ilmenau, Germany.

出版信息

Phys Chem Chem Phys. 2011 Jan 21;13(3):1174-81. doi: 10.1039/c0cp01064b. Epub 2010 Nov 12.

Abstract

Radiation induced degradation effects are studied for a model ionic liquid (IL)--[EMIm]Tf(2)N--in order to distinguish in which way the results of X-ray based material analysis methods can be falsified by the radiation supplied by typical X-ray sources itself. Photoelectron spectroscopy is commonly used for determining the electronic structure of ionic liquids. Degradation effects, which often occur e.g. in organic materials during X-ray or electron irradiation, are potentially critical for the interpretation of data obtained from ionic liquids. The changes of the chemical composition as well as the radiation-induced desorption of 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([EMIm]Tf(2)N) fragments are analysed by X-ray photoelectron spectroscopy (XPS) as well as quadrupole mass spectroscopy (QMS) upon exposure to monochromated or non-monochromated AlKα X-rays from typical laboratory sources. During the irradiation of [EMIm]Tf(2)N, an increasing carbon concentration is observed in both cases and especially the Tf(2)N ion is strongly altered. This observation is supported by the results from the QMS analysis which revealed a variety of different IL fragments that are desorbed during X-ray irradiation. It is shown that the decomposition rate is directly linked to the photon flux on the sample and hence has to be considered when planning an XPS experiment. However, for typical experiments on this particular IL the measurements suggest that the changes are on a larger time scale as typically required for spectra acquisition, in particular if monochromated X-ray sources are used.

摘要

为了区分典型 X 射线源本身提供的辐射会以何种方式伪造基于 X 射线的材料分析方法的结果,研究了模型离子液体(IL)-[EMIm]Tf(2)N 的辐射诱导降解效应。光电电子能谱常用于确定离子液体的电子结构。在 X 射线或电子辐照下,通常会在有机材料中发生降解效应,这些效应可能会对从离子液体中获得的数据的解释产生关键性影响。通过 X 射线光电子能谱(XPS)和四极质谱(QMS)分析暴露于典型实验室源的单色或非单色 AlKα X 射线后化学组成的变化以及[EMIm]Tf(2)N 片段的辐射诱导解吸。在[EMIm]Tf(2)N 的辐照过程中,在两种情况下都观察到碳浓度的增加,特别是Tf(2)N离子发生了强烈的变化。QMS 分析的结果支持了这一观察结果,该结果显示在 X 射线辐照期间解吸了各种不同的 IL 片段。结果表明,分解速率与样品上的光子通量直接相关,因此在规划 XPS 实验时必须考虑到这一点。然而,对于该特定 IL 的典型实验,测量结果表明,在通常需要进行光谱采集的时间尺度上,变化较大,特别是如果使用单色 X 射线源。

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